HRID1876001
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
(3-Bromophenyl)methanamine hydrochloride (3.62 g, 15.64 mmol) and sodium methoxide (3.58 mL, 15.64 mmol) were added to a solution of methyl 2,2-diethoxyacetimidate (5.042 g, 31.3 mmol) in methanol (15 mL). The cloudy mixture was heated at 70 C for 1.5 h and the resulting yellow mixture was concentrated. The residue was purified by silica gel chromatography with 100% ethyl acetate. The desired fractions were concentrated to give a yellow viscous oil (2.5 g, 51%). LCMS: R.T.=2.11; [M+2]+=317.06.
WORKUP
后处理
- temperatureThe cloudy mixture was heated at 70 C for 1.5 h
- concentrationthe resulting yellow mixture was concentrated
- customThe residue was purified by silica gel chromatography with 100% ethyl acetate
- concentrationThe desired fractions were concentrated