Methyl chloroformate → HCID 897069、化合物
反応式
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]=1参加物
5
実験手順
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+).
後処理
- 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
出典と根拠
- ORDレコード
- ord-3cce6c890831493ab91b0eabe8495458
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09133158B2
反応ノート
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