Methyl chloroformate → Methyl (4-bromo-2-fluorobenzyl)carbamate
반응식
Cl[C:2]([O:4][CH3:5])=[O:3].[Br:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][NH2:14])=[C:9]([F:15])[CH:8]=1.C(N(CC)CC)C>C(Cl)Cl>[CH3:5][O:4][C:2](=[O:3])[NH:14][CH2:13][C:10]1[CH:11]=[CH:12][C:7]([Br:6])=[CH:8][C:9]=1[F:15]참가 물질
5
실험 절차
Methyl chloroformate (85.0 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.1 mmol) in methylene chloride (5 mL) at 0° C. After 10 min, the ice-water bath was removed. The mixture was stirred at RT for 1 h, washed with water, and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (220 mg, 83.9%) was directly used in next step without further purification. LCMS: (M+H)=263.9/261.8.
후처리
- customthe ice-water bath was removed
- washwashed with water, and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue (220 mg, 83.9%) was directly used in next step without further purification
출처 및 근거
- ORD 기록
- ord-018cfa94993f48388c9742b39d74a472
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08461330B2
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