HRID1008030

反应详情

EQUATION

反应方程式

HRID 1008030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of of tert-butyl 2-{2-[(2,3-dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]ethoxy}ethylcarbamate (15.34 g, 34.35 mmol) in absolute ethanol (500 mL) was combined with 5% platinum on carbon (12.02 g) in a Parr vessel and placed under hydrogen pressure overnight. The reaction mixture was filtered through a layer of Celite® filter aid. The filtrate was concentrated under reduced pressure. The resulting residue was purified by column chromatography (250 g of silica gel eluting with 1/1 ethyl acetate/hexanes) to provide 11.21 g of tert-butyl 2-{2-[(3-amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]ethoxy}ethylcarbamate.

WORKUP

后处理

  1. custompressure overnight
  2. filtrationThe reaction mixture was filtered through a layer of Celite®
  3. filtrationfilter aid
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was purified by column chromatography (250 g of silica gel eluting with 1/1 ethyl acetate/hexanes)