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

HRID 358986

반응식

HRID 358986 반응식
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]

참가 물질

5

반응물 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)

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1, 4-dihydropyridine, m.p. 145°-147° C.

후처리

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

출처 및 근거

ORD 기록
ord-7e14a53e5d704020aa01189f8f162012
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999362

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