HRID532407

反应详情

EQUATION

反应方程式

HRID 532407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Subsequently, the 3-pentafluorosulfanyl-5-nitrobenzoic acid (5 g) was dissolved in methanol (300 ml), Raney nickel (about 750 mg) was added and hydrogenation was effected under a hydrogen atmosphere (hydrogen balloon). After 3 h, the catalyst was filtered off and the filter residue was washed thoroughly with methanol. The filtrate was concentrated and dried. The residue was purified using silica gel (2×50 g cartridge, n-heptane/EA gradient of 0-100% within 60 min). 3.9 g of the title compound were obtained.

WORKUP

后处理

  1. filtrationthe catalyst was filtered off
  2. washthe filter residue was washed thoroughly with methanol
  3. concentrationThe filtrate was concentrated
  4. customdried
  5. customThe residue was purified
  6. customsilica gel (2×50 g cartridge, n-heptane/EA gradient of 0-100% within 60 min)