氯离子溶液 → (-)-2-(3-Pyridinylmethylthio)methyl-5-cyano-3-carboethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridine

HRID 5648

反应方程式

HRID 5648 反应方程式
[C:1]([C:3]1[CH:4]([C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[CH:21]=2)[C:5]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:6]([CH2:10][S:11][C:12](=N)N)[NH:7][C:8]=1[CH3:9])#[N:2].Cl.ClC[C:32]1[CH:33]=[NH+:34][CH:35]=[CH:36][CH:37]=1.[Cl-].[OH-].[K+]>C1C=CC=CC=1>[N:34]1[CH:35]=[CH:36][CH:37]=[C:32]([CH2:12][S:11][CH2:10][C:6]2[NH:7][C:8]([CH3:9])=[C:3]([C:1]#[N:2])[CH:4]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[CH:21]=3)[C:5]=2[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:33]=1

参与物

6

反应物 4

HCID 312氯离子溶液HCID 14797氢氧化钾HCID 19796447(-)-S-[(5-cyano-3-carboethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridin-2-yl)methyl]isothioureaHCID 214777733-Chloromethylpyridinium hydrochloride

产物 1

HCID 67863868(-)-2-(3-Pyridinylmethylthio)methyl-5-cyano-3-carboethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridine

试剂、催化剂与溶剂 1

HCID 241苯溶剂

实验过程

A mixture of (-)-S-[(5-cyano-3-carboethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridin-2-yl)methyl]isothiourea (mg 500), 3-chloromethylpyridinium hydrochloride (mg 190), benzylthriethylammonium chloride (BTEAC mg 80), KOH (4M, ml 2) and benzene (ml 5) is stirred at room temperature for 15 minutes to separate a precipitate that is filtered and triturated with diethyl ether to give mg 450 of (-)-2-(3-pyridinylmethylthio)methyl-5-cyano-3-carboethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridine.

后处理

  1. customto separate a precipitate that
  2. filtrationis filtered
  3. customtriturated with diethyl ether

来源与证据

ORD记录
ord-88228e4040e04ab3b2c5db9f2b2006b0
来源数据集
uspto-grants-1993_09
专利号
US05245039

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