HRID2289675

反应详情

EQUATION

反应方程式

HRID 2289675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

22.0 g of [(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 2,6-diisopropyl-4-nitro-phenyl ester and 6 g of Raney nickel were mixed in 110 mL tetrahydrofuran under 50 psi of hydrogen. After 21 hours, the reaction was filtered and concentrated to give an orange oil which was dissolved in ethyl acetate, filtered through a pad of silica, and concentrated to give an oily solid. Recrystallization from 53 diethyl ether/hexanes gave 18.60 g (89%) of the title compound as a cream colored solid; mp 153-155° C.

WORKUP

后处理

  1. filtrationthe reaction was filtered
  2. concentrationconcentrated
  3. customto give an orange oil which
  4. filtrationfiltered through a pad of silica
  5. concentrationconcentrated
  6. customto give an oily solid
  7. customRecrystallization from 53 diethyl ether/hexanes