HRID1735641

反应详情

EQUATION

反应方程式

HRID 1735641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Condensed 32.5 g of trifluoromethylsulphenyl chloride was placed in a pressured bottle in a dry ice bath. 60 ml of chilled chloroform was added under nitrogen, followed by the addition of 5.6 g of phenol in 16 g of pyridine and 0.8 g of iron powder. The mixture was stirred in a closed bottle at room temperature for two days. The solution was then washed with water and diluted with hydrochloric acid. After removal of the solvent, the crude product was distilled with a column. The yield was 10 g. The b.p. was 51° C./0.1 mm. NMR (CDCl3), δ 8.1 (s) ppm.

WORKUP

后处理

  1. customwas placed in a pressured bottle in a dry ice bath
  2. washThe solution was then washed with water
  3. additiondiluted with hydrochloric acid
  4. customAfter removal of the solvent
  5. distillationthe crude product was distilled with a column