2-Methoxyethylamine → N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-(2-methoxy)ethyl 2-nitro-1,1-ethenediamine

HRID 850939ノート

反応式

HRID 850939 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].[CH3:22][O:23][CH2:24][CH2:25][NH2:26]>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:26][CH2:25][CH2:24][O:23][CH3:22])=[CH:16][N+:17]([O-:19])=[O:18])[N:9]=1)[CH3:1]

参加物

4

反応物 2

HCID 80182-MethoxyethylamineHCID 678972721-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene

生成物 1

HCID 70482832N-2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl-N'-(2-methoxy)ethyl 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 1.25 g of 1-[2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-1-methylthio-2-nitroethylene, 0.27 g of 2-methoxyethylamine and 20 ml of 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'-(2-methoxy)ethyl 2-nitro-1,1-ethenediamine as an oil.

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-57bf7bf707df431d9f95720033a4c833
出典データセット
uspto-grants-1983_05
特許番号
US04382090

反応ノート

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