Methyl chloroformate → HCID 897069, 화합물
반응식
Cl[C:2]([O:4][CH3:5])=[O:3].[Cl:6][C:7]1[CH:8]=[C:9]([CH2:13][CH2:14][NH2:15])[CH:10]=[CH:11][CH:12]=1.CCN(CC)CC>C(Cl)Cl>[CH3:5][O:4][C:2](=[O:3])[NH:15][CH2:14][CH2:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([Cl:6])[CH:8]=1참가 물질
5
실험 절차
At 0, methyl chloroformate (4.6 g, 48 mmol) was added dropwise to a solution of 2-(3-chloro-phenyl)-ethylamine (5.0 g, 32 mmol) and Et3N (6.4 g, 64 mmol) in DCM (100 mL). After the addition, the mixture was stirred at room temperature for 0.5 hour. The organic layer was washed with water (3×30 mL), 1N HCl (20 mL) and brine (30 mL), dried over anhy. Na2SO4, filtered and concentrated in vacuo. After vacuum drying, the title compound was obtained (6.49 g, 95%) as a white solid. MS: 214.1 (M+H+).
후처리
- additionAfter the addition
- washThe organic layer was washed with water (3×30 mL), 1N HCl (20 mL) and brine (30 mL)
- customdried over anhy
- filtrationNa2SO4, filtered
- concentrationconcentrated in vacuo
- customAfter vacuum drying
출처 및 근거
- ORD 기록
- ord-3cce6c890831493ab91b0eabe8495458
- 출처 데이터셋
- uspto-grants-2015_09
- 특허 번호
- US09133158B2
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