HRID1028944

反应详情

EQUATION

反应方程式

HRID 1028944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromo-3-methylbenzoic acid (2.19 g, 10.18 mmol) in THF (20.37 mL) was treated with N,N′-carbonyldiimidazole (1.98 g, 12.2 mmol). The reaction mixture was stirred at ambient temperature overnight (14 h). Morpholine (3.11 mL, 35.6 mmol) was added in one portion. The resulting solution was stirred for 8 h and then partitioned between EtOAc and water. Organic layer washed with water, dilute HCl, saturated aqueous Na2CO3, water and brine. The solution was then concentrated in vacuo to afford (2-bromo-3-methylphenyl)(morpholino)methanone as a white crystalline solid.

WORKUP

后处理

  1. stirringThe resulting solution was stirred for 8 h
  2. custompartitioned between EtOAc and water
  3. washOrganic layer washed with water, dilute HCl, saturated aqueous Na2CO3, water and brine
  4. concentrationThe solution was then concentrated in vacuo