HRID1735641
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas placed in a pressured bottle in a dry ice bath
- washThe solution was then washed with water
- additiondiluted with hydrochloric acid
- customAfter removal of the solvent
- distillationthe crude product was distilled with a column