1,1-Bis(methylthio)-2-nitroethylene → 1-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene

HRID 236266노트

반응식

HRID 236266 반응식
[CH3:1][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH2:14])[N:9]=1)[CH3:3].[CH3:15][S:16][C:17](SC)=[CH:18][N+:19]([O-:21])=[O:20]>C(#N)C>[CH3:3][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:17]([S:16][CH3:15])=[CH:18][N+:19]([O-:21])=[O:20])[N:9]=1)[CH3:1]

참가 물질

4

반응물 2

HCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 109773182-(Dimethylaminomethyl)-4-(2-aminoethylthiomethyl)thiazole

생성물 1

HCID 678972721-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene수율 53.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

With 2 ml of acetonitrile were mixed 1 g of 2-{[2-(dimethylamino)methyl-4-thiazolyl]methylthio}ethylamine and 1.4 g of 1,1-bis(methylthio)-2-nitroethene, and the resulting mixture was subjected to reaction under reflux for 2 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 5 ml of ethanol was added to the resulting residue, after which the insolubles were removed by filtration. The solvent was removed by distillation under reduced pressure, and the residue thus obtained was purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=20:1 by volume) to obtain 0.8 g (yield 53%) of oily 1-{2-[[2-(dimethylamino)methyl-4-thiazolyl]methylthio]ethylamino}-1-methylthio-2-nitroethene.

후처리

  1. customthe resulting mixture was subjected to reaction
  2. temperatureunder reflux for 2 hours
  3. customAfter completion of the reaction
  4. customthe solvent was removed by distillation under reduced pressure, and 5 ml of ethanol
  5. additionwas added to the resulting residue
  6. customafter which the insolubles were removed by filtration
  7. customThe solvent was removed by distillation under reduced pressure
  8. customthe residue thus obtained
  9. customwas purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=20:1 by volume)

출처 및 근거

ORD 기록
ord-52c8579f4eee4b8ea5835ef33b6e1536
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643849

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