Triethylamine → HCID 21461086、化合物

HRID 2259528ノート

反応式

HRID 2259528 の反応式
[C:1](Cl)(Cl)=[S:2].[CH2:5]([N:7]([CH2:14][CH2:15][CH2:16][NH2:17])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:6].C(N(CC)CC)C>C(Cl)Cl>[CH2:5]([N:7]([CH2:14][CH2:15][CH2:16][N:17]=[C:1]=[S:2])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[CH3:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 3152197N-(3-Aminopropyl)-N-ethyl-N-phenylamine

生成物 1

HCID 21461086HCID 21461086、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
20 °C

実験手順

A solution of thiophosgene (7.43 ml) in CH2Cl2 (300 ml) was added dropwise over 11/2 hours at 20° C. under a nitrogen atmosphere to a stirred solution of N-ethyl-N-(3-aminopropyl)aniline (17.8 g) and triethylamine (27.8 ml) in CH2Cl2 (500 ml). The mixture was stirred at 20° C. for a further 1/2 hours then heated under reflux for 11/2 hours. The mixture was allowed to cool, washed with water, dried over MgSO4, filtered and solvent removed from the filtrate in vacuo. The product was purified by chromatography on silica gel eluting with CH2Cl2 to give N-ethyl-N-(3-isothiocyanatopropyl)aniline (7.2 g) as a red oil.

後処理

  1. temperaturethen heated
  2. temperatureunder reflux for 11/2 hours
  3. temperatureto cool
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customsolvent removed from the filtrate in vacuo
  8. customThe product was purified by chromatography on silica gel eluting with CH2Cl2

出典と根拠

ORDレコード
ord-9b64d9e09ec749d4a9b76a41a0406832
出典データセット
uspto-grants-1995_12
特許番号
US05474580

反応ノート

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