HRID403298

反应详情

EQUATION

反应方程式

HRID 403298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-trifluoromethyl-benzo[b]thiophene-2-carboxylic acid 14a (2.031 mmol, 0.50 g) in THF (8 mL) at −70° C. was treated with a 1.6 M solution of n-BuLi in hexanes (2.66 mL, 4.26 mmol). After 1 h at −70° C., N-fluorobenzenesulfonimide (0.833 g, 2.64 mmol) in THF (2 mL) was slowly added and the reaction was warmed to room temperature. After 1 h the mixture was partitioned between dilute aqueous HCl and EtOAc. The organic layer was washed with water and brine and then concentrated. The residue was triturated with CH2Cl2. The off-white precipitate was collected by filtration to provide compound 14b.

WORKUP

后处理

  1. customAfter 1 h the mixture was partitioned between dilute aqueous HCl and EtOAc
  2. washThe organic layer was washed with water and brine
  3. concentrationconcentrated
  4. customThe residue was triturated with CH2Cl2
  5. filtrationThe off-white precipitate was collected by filtration