HRID1097864

反应详情

EQUATION

反应方程式

HRID 1097864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Chloro-4-(trifluoromethyl)-benzeneacetic acid (3 g) [CAS Reg. No. 601513-26-2] was dissolved in DCM (30 mL) and methyl chloroformiate (1.18 g, 0.97 mL) followed by triethylamine (1.4 g, 1.93 mL) were added drop by drop. To the mixture was added DMAP (0.154 g) and the yellow mixture was allowed to stir for 1 hour at 0° C. A clear solution was obtained. The mixture was diluted with DCM (30 mL) and was poured into sat. NH4Cl solution. The layers were separated and the aqueous phase was further extracted with 2 portions of DCM. The organic layers were washed with brine, dried over Na2SO4 and evaporated to give the title compound (3.0 g) that was used without further purification. NMR (□, CDCl3): 7.6-7.4 (m, 3H); 3.84 (s, 2H); 3.74 (s, 3H).

WORKUP

后处理

  1. additionwere added drop by drop
  2. customA clear solution was obtained
  3. customThe layers were separated
  4. extractionthe aqueous phase was further extracted with 2 portions of DCM
  5. washThe organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. customevaporated