Aziridine → HCID 67897156、化合物

HRID 236260

反応式

HRID 236260 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]2[O:13][C:12](=[CH:14][N+:15]([O-:17])=[O:16])[NH:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.[CH3:18][N:19]([CH2:21][C:22]1[S:26][C:25]([CH2:27][SH:28])=[CH:24][C:23]=1[CH3:29])[CH3:20].[CH2:30]1[NH:32][CH2:31]1>C(Cl)Cl.CO>[CH3:20][N:19]([CH2:21][C:22]1[S:26][C:25]([CH2:27][S:28][CH2:30][CH2:31][NH:32][C:12]([NH:11][CH2:10][CH:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)[OH:13])=[CH:14][N+:15]([O-:17])=[O:16])=[CH:24][C:23]=1[CH3:29])[CH3:18]

参加物

6

反応物 3

HCID 9033AziridineHCID 13825272HCID 13825272、化合物HCID 67897164HCID 67897164、化合物

生成物 1

HCID 67897156HCID 67897156、化合物収率 83.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒3 回HCID 6344Dichloromethane溶媒

実験手順

In a mixed solvent of 20 ml of methylene chloride and 10 ml of methanol was dissolved 2.4 g of 5-(3-methoxyphenyl)-2-nitromethyleneoxazolidine at room temperature, and a solution of 2.0 g of 5-(dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene in 5 ml of methanol was added thereto in a nitrogen atmosphere. Then, the solution of 0.5 g of ethyleneimine in 5 ml of methanol was added dropwise at the same temperature over a period of 10 minutes. After addition, the resulting solution was subjected to reaction with stirring for 5 hours. After the completion of the reaction, the solvent was removed by distillation under reduced pressure, and the residue obtained was purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=30:1 by volume) to obtain 4.0 g (yield 83.5%) of oily N-{2-[[5-(dimethylamino)methyl-4-methyl-2-thienyl]methylthio]ethyl}-N'-[2-(3-methoxyphenyl)-2-hydroxyethyl]-2-nitro-1,1-ethenediamine.

後処理

  1. additionAfter addition
  2. customthe resulting solution was subjected to reaction
  3. customAfter the completion of the reaction
  4. customthe solvent was removed by distillation under reduced pressure
  5. customthe residue obtained
  6. customwas purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=30:1 by volume)

出典と根拠

ORDレコード
ord-963b92fb10944371ba15777abffa5a54
出典データセット
uspto-grants-1987_02
特許番号
US04643849

関連ノート

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