HRID1512038

反应详情

EQUATION

反应方程式

HRID 1512038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a solution of 5-chlorosalicylaldehyde (5 g, 32 mmol) in N,N-dimethylformamide (100 mL) was added 2-bromo-2-methyl-propionic acid tert-butyl ester (10.7 g, 48 mmol), Cs2CO3 (3.1 g, 95 mmol). The reaction mixture was heated at 140° C. for 18 h. The mixture was partitioned between ethyl acetate and water. The organic layer was separated, and aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water, brine, dried over Na2SO4 and concentrated to give 2-(4-chloro-2-formyl-phenoxy)-2-methyl-propionic acid tert-butyl ester as a pale yellow solid (Yield 5.2 g, 54%)

WORKUP

后处理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. customThe organic layer was separated
  3. extractionaqueous layer was extracted with ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated