Acetic Acid → 2-Mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine

HRID 1493305

反応式

HRID 1493305 の反応式
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].[SH2:29].C([N+](CCCC)(CCCC)CCCC)CCC.CC(O)=O>C(Cl)Cl>[SH:29][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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 3064723Diethyl 2-(chloromethyl)-6-methyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylateHCID 162054371-Butanaminium,N,N,N-tributyl-, sulfide (1:1)

生成物 1

HCID 116758332-Mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine収率 70.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 2-chloromethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine (1 g) and tetrabutylammonium hydrogen sulfide (0.7 g) in methylene chloride (10 ml) is stirred at -10° C., for 20 minutes, neutralized with a drop of AcOH, evaporated under vacuum and the residue recrystallized from Et2O to give 0.7 g of 2-mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine, m.p. 145°-147° C.

後処理

  1. customevaporated under vacuum
  2. customthe residue recrystallized from Et2O

出典と根拠

ORDレコード
ord-0b934954ba874e34b854e3cbdf3d7c28
出典データセット
uspto-grants-1991_06
特許番号
US05021436

関連ノート

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