HRID1876001

反应详情

EQUATION

反应方程式

HRID 1876001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe cloudy mixture was heated at 70 C for 1.5 h
  2. concentrationthe resulting yellow mixture was concentrated
  3. customThe residue was purified by silica gel chromatography with 100% ethyl acetate
  4. concentrationThe desired fractions were concentrated