Cyclopropylamine → N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine

HRID 1200247ノート

反応式

HRID 1200247 の反応式
[CH3:1][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15](SC)=[CH:16][N+:17]([O-:19])=[O:18])[N:9]=1)[CH3:3].[CH:22]1([NH2:25])[CH2:24][CH2:23]1>C(O)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:15]([NH:25][CH:22]2[CH2:24][CH2:23]2)=[CH:16][N+:17]([O-:19])=[O:18])[N:9]=1)[CH3:1]

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 678972721-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene

生成物 1

HCID 70363512N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A reaction mixture, prepared from 1-[2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene, cyclopropylamine and ethanol, was heated to refluxing temperature for about three hours. The solvent was then removed by evaporation and the resulting residue was chromatographed over silica using a gradient elution technique. The desired compound was eluted with a 5:95 methanol:ethyl acetate solvent mixture. Removal of the solvent yielded N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-cyclopropyl 2-nitro-1,1-ethenediamine which melted at 128.5°-131.5° C. after recrystallization from a methanol/ethyl acetate solvent mixture.

後処理

  1. temperaturewas heated
  2. temperatureto refluxing temperature for about three hours
  3. customThe solvent was then removed by evaporation
  4. customthe resulting residue was chromatographed over silica using
  5. washa gradient elution technique
  6. washThe desired compound was eluted with a 5:95 methanol
  7. customRemoval of the solvent

出典と根拠

ORDレコード
ord-2cca6b5a100f4a8892a8feaed54955d1
出典データセット
uspto-grants-1990_02
特許番号
US04904792

反応ノート

読み込み中…