2-Chlorobenzylamine → 1-Chloro-2-(isocyanatomethyl)benzene

HRID 650102

반응식

HRID 650102 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].Cl[C:11](Cl)([O:13]C(=O)OC(Cl)(Cl)Cl)Cl.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][N:5]=[C:11]=[O:13]

참가 물질

6

반응물 3

HCID 666482-ChlorobenzylamineHCID 94429TriphosgeneHCID 516892Sodium Bicarbonate

생성물 1

HCID 27333671-Chloro-2-(isocyanatomethyl)benzene수율 232.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-chlorobenzylamine (1.0 g, 7.06 mmol) in a mixture of CH2Cl2 and H2O (10 mL/10 mL), triphosgene (838 mg, 2.82 mmol) and NaHCO3 (1.78 g, 21.2 mmol) were added. The reaction mixture was stirred at room temperature for 16 hours. Then the reaction mixture was partitioned between CH2Cl2 and water. The combined organic layers are dried over MgSO4 and filtered. The solvent was evaporated to give the desired product (1.1 g, 93%). EI-MS m/z 168.7 (M+).

후처리

  1. additionwere added
  2. customThen the reaction mixture was partitioned between CH2Cl2 and water
  3. dry with materialThe combined organic layers are dried over MgSO4
  4. filtrationfiltered
  5. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-291c8d96be1d44cfb70e9e6690479ef3
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271261B1

연결된 노트

불러오는 중…