小叶臭黄皮中单萜和倍半萜类成分研究

研究小叶臭黄皮Clausena excavata茎和叶甲醇提取物的单萜和倍半萜类成分。小叶臭黄皮茎和叶提取物的乙酸乙酯部位经硅胶、RP-18和HPLC等色谱技术分离纯化,通过理化常数和波谱数据鉴定化合物的结构。从小叶臭黄皮茎和叶中分离得到10个化合物,分别鉴定为:1个单萜,命名为excamonoterpene(1);9个倍半萜,即(6R,9S)-9,10-dihydroxy-4-megastigmen-3-one(2),(3R,6R,7E)-3-hydroxy-4,7-megastigmadien-9-one(3),(3S)-3-hydroxy-7,8-dihydro-β-ionone(4),(3S,5R,6S)-3-hydroxy-5,6-epoxy-β-ionone(5),(6R,9R)-9-hydroxy-4-megastigmen-3-one(6),(3S,5R)-dihydroxy-6,7-megstigmadien-9-one(7),(-)-loliolide(8),caryolane-1,9α-diol(9),2,6-dihydroxyhumula-3(12),7(13),9(E)-triene(10)。化合物1为1个新的单萜,2~10为首次从该种植物中分离得到。     

朝天罐根化学成分的研究

目的:研究朝天罐Osbeckia opipara根化学成分.方法:通过多种柱色谱方法进行分离纯化,根据化合物的理化性质和光谱数据进行结构鉴定.结果:从朝天罐根的甲醇提取物中分离得到12个化合物:lasiodiplodin(1),de-O-methyllasiodiplodin(2),2,3-dihydro-2-hydroxy-2,4-dimethyl-5-trans-propenylfuran-3-one(3),integracin(4),5α,8α-epidioxy-(22E,24R)-ergosta-6,22-dien-3β-ol(5),3,3',4'-tri-O-methylellagic acid(6),5-羟甲基糠醛(7),吐叶醇(8),白桦脂酸(9),2α-羟基乌索酸(10),(24R)-stigmast-4-ene-3-one(11),eugenitin(12).结论:所有化合物均为首次从该植物中分离得到.     

海南血竭的化学成分(英文)

目的:对海南龙血树所产血竭的化学成分进行研究。方法:运用硅胶柱色谱和SephadexLH-20凝胶柱色谱等方法对化合物进行分离纯化,通过理化性质及波谱数据鉴定其结构。结果:分离鉴定了8个化合物,分别为丁香脂素(1),松脂醇(2),蛇菰宁(3),2-(4-hydroxyphenyl)-6-(3-methoxy-4-hydroxyphenyl)-3,7-dioxabicyclo[3.3.0]octane(4),5,7-二羟基-4′-甲氧基-8-甲基黄烷(5),7,4′-二羟基-8-甲氧基高异黄烷(6),(2R)-7,4′-二羟基-8-甲基黄烷(7),(2S)-7,3′-二羟基-4′-甲氧基黄烷(8)。结论:以上化合物均为首次从海南血竭分离得到。     

瓦山安息香树皮中四氢呋喃型木脂素类成分

目的:研究瓦山安息香树皮中木脂素类成分。方法:采用反复硅胶柱色谱和葡聚糖凝胶柱色谱的色谱方法结合波谱方法分离鉴定瓦山安息香树皮的化学成分。结果:从瓦山安息香树皮提取物的醋酸乙酯萃取部位和三氯甲烷部位中分离得到8个四氢呋喃型木脂素类化合物,1个苯并呋喃型木脂素和1个丁烷型木脂素。根据化合物的波谱数据鉴定化合物的结构为(-)-(2R,3R)-secoisolariciresinol(1),2R,3S-dihydrodehydrodiconiferyl alcohol(2),罗汉松脂醇(3),(±)-salicifoliol(4),(-)-epipinoresinol(5),lariciresinol-4'-monomethy ether(6),(+)-pinoresinol monomethy ether(7),piperitol(8),styraxin(9),1R,2R,5S,6R-2-(4'-hydroxy-3'-methoxyphenyl)-6-(3″,4″-dimethoxyphenyl)-3,7-dioxabicyclo[3.3.0]octane 4'-O-β-D-glucopyranoside(10)。结论:6个化合物(1,4,6,7,8,10)首次从安息香属植物中分离的得到。     

贯叶金丝桃化学成分研究

目的:研究贯叶金丝桃Hypericum perforatum的化学成分。方法:通过各种柱色谱进行分离纯化,根据理化性质和波谱数据对所得化合物进行结构鉴定;测定化合物对基因重组人PTP1B的抑制率。结果:从中分离并鉴定了10个化合物:D-甘露醇(1),邻苯二甲酸二异丁酯(2),(7E,6R,9S)-9-hydroxy-4,7-megastigmadien-3-one(3),(6S,9R)-roseoside(4),2,6-dim-ethoxy-4-hydroquinone-1-O-β-D-glucopyranoside(5),2,6-dimethoxy-4-hydroxybenzyl alcohol 1-O-β-D-glucopyranoside(6),syringate4-O-β-glucopyranoside(7),金丝桃素(8),skyrin-6-O-β-D-glucopyranoside(9),(R)-3,4-二羟基-苯甲酸-1’-丙三醇酯(10)。在2μmol.L-1时,化合物9对基因重组人PTP1B的抑制率为96.4%,IC50为2.5μmol.L-1。结论:化合物10为新化合物,化合物2～4,7为首次从该属中分离得到,化合物5,6从该植物中首次得到。体外活性筛选表明化合物8具有显著的PTP1B抑制作用。     

中药桂枝化学成分研究

该文对桂枝中的化学成分进行了研究。采用硅胶柱色谱、凝胶(Sephadex LH-20)柱色谱、制备高效液相色谱等方法分离纯化桂枝中的化学成分,并根据波谱数据进行结构鉴定。从中分离鉴定了22个化合物,分别为dihydrorosavin(1),rosavin(2),1-phenyl-propane-1,2,3-triol(3),patchoulol(4),graphostromane B(5),(+)-lyoniresinol-3a-O-β-D-glucopyranoside(6),(-)-lyoniresinol-3a-O-β-D-glucopyranoside(7),cinnacaside(8),subaveniumin A(9),3-phenyl-2-propenyl-6-O-L-arabinopyranosyl-β-glucopyranoside(10),2-phenylethyl-β-vicianoside(11),cinnacasol(12),[(2R,3S,4S,5R,6R)-6-(benzyloxy)-3,4,5-trihydroxytetrahydro-2H-pyran-2-yl]methyl hydrogen sulfate(13),coniferyl aldehyde(14),(2R,3R)-5,7-dimethoxy-3′,4′-methylenedioxyflavan-3-ol(15),cinnacassin L(16),E-cinnamic alcohol(17),(E)-3-(2-methoxyphenyl)-2-propen-1-ol(18),2-hydroxyphenylpropanol(19),cinnamomulactone(20),(+)-syringaresinol(21)和cinnamomumolide(22)。其中化合物1为新化合物,3～7,9～11,13,15,18及19均为首次从桂枝中分离得到。     

昆明柏化学成分研究

目的:研究昆明柏Sabina gaussenii枝叶中的化学成分。方法:应用硅胶,羟丙基葡聚糖凝胶(Sephadex LH-20),RP-18,MCI-gel柱色谱和半制备HPLC等手段进行分离纯化;根据理化性质和波谱学方法鉴定化合物的结构。结果:从昆明柏枝叶乙醇提取物的乙酸乙酯萃取部位中分离得到7个化合物,分别鉴定为(7S,8R)-dihydro-3-hydroxy-8-hydroxy-methyl-7-(4-hydroxy-3-methoxyphenyl)-1-benzofuranpropanol(1),(8R,8'S,7S)-4'-(3″-methoxyrhamnopyranosyl)oxy-8'-hydroxy-3,3',4-trimethoxy-8-hydroxymethyl-lign-7-9'-lactone(2),7S,8R-erythro-4,7,9,9'-tetrahydroxy-3,3'-dimethoxy-8-O-4'-neolignan(3),7S,8Sthreo-4,7,9,9'-tetrahydroxy-3,3'-dimethoxy-8-O-4'-neolignan(4),leucoseceptoside A(5),焦地黄苯乙醇苷D(6),blumenol A(7)。结论:化合物1~7均为首次从该植物中分离得到。     

紫花前胡中化学成分的研究

采用HP20大孔吸附树脂、ODS、硅胶柱色谱、Sephadex LH-20柱色谱和半制备HPLC等色谱分离手段对紫花前胡的化学成分进行研究。结合理化性质及MS,NMR等谱学数据鉴定化合物的结构,从紫花前胡80%乙醇提取物中分离并鉴定了12个化合物,分别是(9R,10R)-9-acetoxy-8,8-dimethyl-9,10-dihydro-2H,8H-benzo[1,2-b:3,4-b']dipyran-2-one-10-yl ester(1)、补骨脂呋喃香豆精(2)、顺式-3',4'-二千里光酰基-3',4'-二氢邪蒿内酯(3)、(3'R,4'R)-3'-angeloyloxy-4'-senecioyloxy-3',4'-dihydroseselicalipteryxin(4)、(+)-8,9-dihydro-8-(2-hydro-xypropan-2-yl)-2-oxo-2H-furo[2,3h]chromen-9-yl-3-methylbut-2-enoate(5)、libanoridin(6)、丝立尼亭(7)、花椒素(8)、crocatone(9)、peujaponisinol B(10)、peujaponisinol A(11)、ostenol(12)。其中,化合物1~5为首次从当归属植物中分离得到,化合物7~12为首次从紫花前胡中分离得到。     

短舌紫菀化学成分及生物活性的研究

目的:对短舌紫菀Aster sampsonii全草的化学成分进行研究。方法:以甲醇-石油醚-乙醚1∶1∶1提取,用氯仿进行萃取,对氯仿部位采用各种柱色谱进行分离纯化,通过波谱数据分析(MS,NMR,HMBC等)进行结构鉴定,并对部分化合物进行生物活性实验。结果:分离鉴定了10个化合物,分别为(4αR,4′αR,5S,5′S,9αR,9′αR)-4,4′,4α,4′α,5,5′,6,6′,7,7′,8,8′-dodecahydro-3,3′,4α,4′α,5,5′-hexamethyl-2H,2′H-9α,9′α-binaphtho[2,3-b]furan-2,2′-dione(1),furanoligularenone(2),(4αR,5S,8αR)-4α,5,6,7,8,8α-hexahydro-8α-hydroxy-3,4α,5-trimethylnaphtho[2,3-b]furan-2(4H)-one(3),(4αR,5S,8αS)-4α,5,6,7,8,8α-hexahydro-8α-hydroxy-3,4α,5-trimethylnaphtho[2,3-b]furan-2(4H)-one(4),methyl 1′-hydroxy-2′,6′-dimethoxy-4′-oxocyclohexanacetate(5),1′-hydroxy-2′-methoxy-4′-oxocyclohexanacetate methyl(6),loliolide(7),jacaranone(8),β-谷甾醇(9),木栓酮(10),生物活性筛选结果表明化合物3对金黄色葡萄球菌有弱的抑制作用。结论:其中化合物1~8为首次从该属植物中分离得到。     

苍术聚炔类化学成分研究

目的研究苍术中聚炔类化学成分。方法采用开放ODS柱色谱及制备液相色谱等分离技术,根据化合物的理化性质和光谱数据鉴定其结构。结果从苍术80%乙醇提取物部分共分离7个聚炔类成分,分别鉴定为12,14-diacetate-2E,8E,10E-trien-4,6-diyn-1-ol(1),(2Z,4E,10E)-dodeca-2,4,10-trien-6,8-diynyl acetate(2),(5E,11E)-trideca-1,5,11-trien-7,9-diyne-3,4-diyl diacetate(3),1-(2-Furvl)-(E)-nonene-3,5-diyne-l,2-diacetate(4),atractulodin(5),(4E,6E,12E)-tetradecatriene-8,10-diyne-1,3-diol-diacetate(6),atractylodinol(7)。结论化合物1,2鉴定为苍术新的聚炔类成分。     

Phytotoxic compounds from Prionosciadium watsoni

Bioassay-guided fractionation of a phytotoxic extract of Prionosciadium watsoni led to the isolation of three new pyranocoumarins and two pyranochromones. The new compounds were characterized as propionic acid (9R,10R)-9-acetoxy-8,8-dimethyl-9,10-dihydro-2H,8H-benzo[1,2-b:3,4-b']dipyran-2-one-10-yl ester (1), isobutyric acid (9R,10R)-9-hydroxy-8,8-dimethyl-9,10-dihydro-2H,8H-benzo[1,2-b:3,4-b']dipyran-2-one-10-yl ester (2), isobutyric acid (9R)-8,8-dimethyl-9,10-dihydro-2H,8H-benzo[1,2-b:3,4-b']dipyran-2-one-9-yl ester (10), 2-methylbut-(2Z)-enoic acid (3R)-5-methoxy-3,4-dihydro-2,2,8-trimethyl-6-oxo-2H,6H-benzo[1,2-b:5,4-b']dipyran-3-yl ester (11), and isobutyric acid (3R)- 5-methoxy-3,4-dihydro-2,2,8-trimethyl-6-oxo-2H,6H-benzo[1,2-b:5,4-b']dipyran-3-yl ester (12) by spectroscopic and chemical methods. The stereochemistry at the stereogenic centers was established by applying the Mosher ester methodology. The structures of 1 and 2 were corroborated by single-crystal X-ray diffraction studies. The phytotoxic activity of the isolated compounds was assessed on Amaranthus hypochondriacus, Echinochloa crus-galli, and Lemna pausicostata. The phytotoxins also modified the electrophoretic mobility of calmodulin from both bovine-brain and spinach.     

慈竹茹中木脂素类化学成分的研究

通过硅胶、大孔树脂、葡聚糖凝胶Sephadex LH-20和HPLC等多种色谱分离方法相结合,从慈竹茹Sinocalamusafinis茎的乙醇提取物的乙酸乙酯萃取部分中分离得到15个化合物;借助理化性质和波谱学数据分析,鉴定其结构为(+)-(1S,2R)-1,2-双(4-羟基-3-甲氧基苯基)-1,3-丙二醇(1),苏式-愈创木基甘油-β-O-4’-松柏基醚(2),赤式-愈创木基甘油-β-O-4’-松柏基醚(3),(+)-(7S,8R,8’R)-5’-甲氧基落叶松树脂醇(4),(+)-(7S,8R,8’R)-5,5’-二甲氧基落叶松树脂醇(5),(±)-秃毛冬青素Ⅰ(6),(-)-丁香树脂酚(7),(-)-杜仲树脂酚(8),(-)-(8R,8R’)-4,4’-二羟基-3,3’,5,5’-四甲氧基木脂烷-9,9’-二醇(9),(-)-开环异落叶松树脂酚-9,9’-缩丙酮(10),(+)-珍珠花树环木脂醇(11),2,6-二甲氧基吡喃-4-酮(12),β-谷甾醇(13),4-羟基桂皮酸(14)和2,6-二甲氧基对苯醌(15)。这些化合物均为首次从慈竹属植物中分离得到,其中化合物12为新天然产物。     

New naphthopyranone glycosides from Paepalanthus vellozioides and Paepalanthus latipes.

Three new compounds-3, 4-dihydro-10-hydroxy-7-methoxy-3-(R)-methyl-1H-3,4-dihydronaphtho- ]2, 3c]-pyran-1-one-9-O-beta-D-glucopyranoside (1), 3, 4-dihydro-10-hydroxy-7-methoxy-3-(R)-methyl-1H-3,4-dihydronaphtho- [2, 3c]-pyran-1-one-9-O-beta-D-glucopyranosyl-(1-->6)-glucopyranoside (2), and 3,4-dihydro-10-dihydroxy-7-methoxy-3-(R)-methyl-1H-3, 4-dihydronaphtho-[2,3c]-pyran-1-one-9-O-beta-D-allopyranosyl (1-->6)glucopyranoside (3)-were isolated from the leaves of Paepalanthus vellozioides and Paepalanthus latipes and characterized by spectrometric methods, mainly electrospray mass spectrometry and 1D and 2D NMR experiments. These unusual glycosylated dihydronaphthopyranones may serve as taxonomic markers of the genus Paepalanthus, since these compounds were not detected in other genera belonging to the Eriocaulaceae family.     

桑椹醇提物的化学成分研究

目的研究桑椹Mori Fructus醇提物的化学成分。方法采用硅胶、Sephadex LH-20和ODS柱色谱法及半制备型高效液相色谱进行分离纯化,通过其理化性质和波谱数据对化合物结构进行鉴定。结果从桑椹醇提物中分离得到12个化合物,分别鉴定为桑脂素苷(1)、(7R,8S)-4,7,9,9′-tetrahydroxy-3,3′-dimethoxy-8-O-4′-neolignan-9′-O-β-D-glucopyranoside(2)、2-苯乙基-β-D-吡喃葡萄糖苷(3)、1′-O-苯乙基-β-D-呋喃芹菜糖基-(1→2)-β-D-吡喃葡萄糖苷(4)、苯甲醇-O-β-D-吡喃葡萄糖苷(5)、过氧麦角甾醇(6)、(24R)-6β-hydroxy-24-ethyl-cholest-4-en-3-one(7)、(22E)-5α,8α-epidioxy-24-methyl-cholesta-6,9(11),22-trien-3β-ol(8)、trans-(S)-(+)-脱落酸(9)、cis-(S)-(+)-脱落酸(10)、(S)-(+)-1-甲基-脱落-6-酸(11)、菜豆酸(12)。结论化合物1为未见文献报道的新化合物,化合物2、7~12为首次从该植物中分离得到。     

阔带凤丫蕨倍半萜类化学成分研究

目的:研究阔带凤丫蕨的化学成分。方法:采用色谱法进行分离,根据理化性质和波谱数据鉴定化合物的结构。结果:分离得到15个化合物,包括10个倍半萜类化合物,分别是(3S)-蕨苷D(1),表蕨素L(2),蕨素D(3),金粉蕨亭(4),蕨素Z(5),onitisin(6),onitisin-glucopyranoside(7),onitin-15-O-β-D-glucopyranoside(8),(2S,3R)-pterosin-L-2’-O-β-D-glucopyrano-side(9),(3R)-peterosin D-3-O-β-D-glucopyranoside(10),其他化合物分别是尿嘧啶(uracil,11),3,4-二羟基苯甲醛(3,4-di-hydroxybenzaldehyde,12),5-羟甲基糠醛(5-hydroxymethyl-2-furancarboxaldehyde,13),β-谷甾醇(β-sitosterol,14),胡萝卜苷(dau-costerol,15)。结论:以上15个化合物均为首次从阔带凤丫蕨中分离得到,其中9个化合物首次从凤丫蕨属中得到。     

Cytotoxic constituents of the roots of Ekmanianthe longiflora

Bioactivity-directed fractionation of the CHCl(3) extract of the roots of Ekmanianthe longiflora resulted in the isolation of three new natural products, (2R,3R,4R)-3,4-dihydro-3, 4-dihydroxy-2-(3-methyl-2-butenyl)-1(2H)-naphthalenone (1), (2S,3R, 4R)-3,4-dihydro-3, 4-dihydroxy-2-(3-methyl-2-butenyl)-1(2H)-naphthalenone (2), and (2R, 3aR,9R,9aR)-9-hydroxy-2-(1-hydroxy-1-methylethyl)-2,3,3a,4,9 , 9a-hexahydro-naphtho[2,3-b]furan-4-one (3), together with the known compounds 2-(1-hydroxyethyl)naphtho[2,3-b]furan-4,9-quinone (4), 2-acetylnaphtho[2,3-b]furan-4,9-quinone (5), dehydro-iso-alpha-lapachone (6), alpha-lapachone (7), catalponol, and epi-catalponol. The structures of 1-3 were determined using a combination of NMR spectroscopic techniques, and the absolute configurations of compounds 1 and 2 were obtained using Mosher ester methodology. Compounds 4-6 showed significant cytotoxicity in a panel of human cancer cells. alpha-Lapachone (7) exhibited only marginal activity, and catalponol and epi-catalponol were inactive in this regard. When tested at 72 mg/kg/injection in an in vivo mouse P-388 leukemia system, compound 4 was inactive (110% T/C).     

New antioxidant hydroquinone derivatives from the algicolous marine fungus Acremonium sp

A marine fungal isolate, identified as Acremonium sp., was mass cultivated and found to produce two novel hydroquinone derivatives, 7-isopropenylbicyclo[4.2.0]octa-1,3,5-triene-2,5-diol (1) and 7-isopropenylbicyclo[4.2.0]octa-1,3,5-triene-2,5-diol-5-beta-D-glucopyranoside (2). Compound 1 and its glucoside 2 possess a most unusual ring system. The new natural products (3R,4S)-3,4-dihydroxy-7-methyl-3,4-dihydro-1(2H)naphthalenone (3) and (3S,4S)-3,4-dihydroxy-7-methyl-3,4-dihydro-1(2H)-naphthalenone (4) were obtained as a 1:0.8 mixture. 2-(1-Methylethylidene)pentanedioic acid (5) was isolated for the first time as a natural product and its structure proven by X-ray analysis. In addition to these compounds an inseparable mixture of three new isomeric compounds, pentanedioic acid 2-(1-methylethylidene)-5-methyl ester (6), pentanedioic acid 2-(1-methylethylidene)-1-methyl ester (7), and pentanedioic acid 2-(1-methylethenyl)-5-methyl ester (8), was also obtained. Isolated together with the new compounds were three known hydroquinone derivatives, 9, 10, and 11. The structures of all compounds were determined by interpretation of their spectroscopic data (1D and 2D NMR, MS, UV, and IR). Each isolate was tested for its antioxidant properties, and compounds 1 and 9-11 were found to have significant activity.     

Phelligridins C-F: cytotoxic pyrano[4,3-c][2]benzopyran-1,6-dione and furo[3,2-c]pyran-4-one derivatives from the fungus Phellinus igniarius

Three unique pyrano[4,3-c][2]benzopyran-1,6-dione derivatives and a new furo[3,2-c]pyran-4-one, named phelligridins C-F (2-5), together with hispolon (8), (E)-4-(3,4-dihydroxyphenyl)but-3-en-2-one (9), 4-hydroxybenzaldehyde, protocatechualdehyde, syringic acid, protocatechuic acid, caffeic acid, isoergosterone, and octadecyl ferulate were isolated and identified from the ethanolic extract of Phellinus igniarius. Their structures were determined by spectroscopic methods including IR, MS, and 1D and 2D NMR experiments. The structures of the new compounds were characterized as 3-(4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (2), 3-(3,4-hydroxystyryl)-8,9-dihydroxypyrano[4,3-c]isochromene-4-one (3), 8,9-dihydroxy-3-[5',6'-dihydroxy-5' '-methyl-3' '-oxo-spiro[fural-2' '(3' 'H),1'-indene]-2'-yl]-1H,6H-pyrano[4,3-c][2]benzopyran-1,6-dione (4), and (3Z)-3-(3,4-dihydroxybenzylidene)-6-(3,4-dihydroxystyryl)-2,3-dihydro-2-methoxy-2-(2-oxo-propyl)furo[3,2-c]pyran-4-one (5), respectively. Some compounds including 2 and 3 showed in vitro selective cytotoxicity against a human lung cancer cell line (A549) and a liver cancer cell line (Bel7402). Possible biogenetic sequences to the formation of 1-9 are postulated.     

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??OBJECTIVE To study the chemical constituents of Rhizoma Zingiberis. METHODS Diaion HP-20, Toyopearl HW-40, ODS, silica gel column and semi-preparation liquid were used to separate and purify the structure, and the structure was identified according to the physical and chemical properties and spectral data of the compound. RESULTS Fifteen compounds were isolated and identified from Rhizoma Zingiberis, which were renealtin A(1),kravanhol A(2),1, 7-bis(3,4-di-hydroxyphenyl)-3-heptanone(3),dihydrocannabinone C(4), 1, 7-bis(3, 2), 1, 7-bis(3,4-di-hydroxyphenyl) 4-dihydroxyphenyl) heptane-3-ylacetate(5),(5R)-1,7-bis(3, 4-dihydroxy)-3-hydroxyphenylheptane(6), citrus acid(7), citrate 4-(1-methoxyethyl)-phenol(8), 3-indolecarboxy(9), 3, 4-dimethoxyphenylacetic acid(10),(2E,6E)-2,6-dimethylocta-2, 6-dienedioicacid(11), cyclo-(D-Leu-L-Trp)(12), cyclo-(S-Pro-S-Phe)(13), 8-hydroxygeraniol(14) and (Z)-2, 6-dimethyloct-6-ene-1, 8-dihydroxy(15). CONCLUSION Compounds 1-15 were isolated from the plant for the first time.