Triethylamine → HCID 21461086, 화합물

HRID 2259528노트

반응식

HRID 2259528 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21461086HCID 21461086, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9b64d9e09ec749d4a9b76a41a0406832
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05474580

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