HRID258192

反应详情

EQUATION

反应方程式

HRID 258192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl α-nitro-9H-thioxanthene-9-acetate (4.4 g, 13.4 mmol) is hydrogenated in 200 mL of ethanol and 13.5 mL of concentrated hydrochloric acid with 1.0 g of 20% palladium on carbon (51 psi, 28 hours). The filtered solution is stripped of solvent and the residual solid washed with dichloromethane, dried at 45° C./2 mm Hg. This gives 3.66 g of the title compound; mp 238°-240° C. An additional crop (0.41 g) is obtained after cooling the mother liquor; mp 233°-236° C.

WORKUP

后处理

  1. washthe residual solid washed with dichloromethane
  2. customdried at 45° C./2 mm Hg
  3. customAn additional crop (0.41 g) is obtained
  4. temperatureafter cooling the mother liquor