反応式
Cl[CH2:2][C:3]1[NH:4][C:5]([CH3:28])=[C:6]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].[S:29]1[CH:33]=[CH:32][CH:31]=[C:30]1[C:34]([O-])=O.[Na+].[CH3:38]CO.COCCOC>C(O)C>[C:30]1([S:34][CH2:2][C:3]2[NH:4][C:5]([CH3:28])=[C:6]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:7]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=3)[C:8]=2[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:38]=[CH:29][CH:33]=[CH:32][CH:31]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 2-chloromethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1, 4-dihydropyridine (5.6 g) in EtOH/DME (5/1; 20 ml) is added dropwise at +10° C. to a stirred solution of sodium thiophenate (1.8 g) in ethanol (10 ml), under N2 atmosphere. After two hours at room temperature the reaction mixture is evaporated under vacuum and the residue is partitioned between Et2O (100 ml) and water (50 ml). The organic phase is washed with a satured solution of sodium bicarbonate (2×20 ml) and water (3×20 ml), dried (Na2SO4) and evaporated to dryness. The residue is recrystallized from isopropylether to give 5.7 g of 2-(phenylthio)methyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1, 4-dihydropyridine, m.p. 92°-94° C.
後処理
- customAfter two hours at room temperature the reaction mixture is evaporated under vacuum
- customthe residue is partitioned between Et2O (100 ml) and water (50 ml)
- washThe organic phase is washed with a satured solution of sodium bicarbonate (2×20 ml) and water (3×20 ml)
- dry with materialdried (Na2SO4)
- customevaporated to dryness
- customThe residue is recrystallized from isopropylether
出典と根拠
- ORDレコード
- ord-ccc369e802704088bd120162c649889f
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US04999362
関連ノート
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