HRID222382

反应详情

EQUATION

反应方程式

HRID 222382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4.2 2.50 g of tert-butyl 3-tert-butoxycarbonylamino-6-ethoxy-7-fluoro-5-nitroindazole-1-carboxylate are hydrogenated in 20 ml of methanol at RT (catalyst: Raney nickel 0.5 g, hydrogen uptake: 300 ml). The reaction batch is filtered and evaporated. Purification of the residue by column chromatography on silica gel (eluent: petroleum ether: ethyl acetate 7:3) gives 3.30 g (36%) of tert-butyl 5-amino-3-tert-butoxycarbonylamino-6-ethoxy-7-fluoroindazole-1-carboxylate, MS-FAB (M+H+)=441.

WORKUP

后处理

  1. filtrationThe reaction batch is filtered
  2. customevaporated
  3. customPurification of the residue by column chromatography on silica gel (eluent: petroleum ether: ethyl acetate 7:3)