HRID639668

反应详情

EQUATION

反应方程式

HRID 639668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methylamine (40% solution in water) (0.055 ml) was added to a solution of (2-amino-6-bromo-3-nitro-pyridin-4-yl)-benzyl-carbamic acid ethyl ester (50 mg) in THF (0.5 ml) at room temperature. The reaction was stirred under nitrogen for 16 hours then the solution pre-absorbed directly onto silica gel. The mixture was purified by chromatography on an Isco Companion, eluting with ethyl acetate:heptane, increasing the gradient linearly from 20:80 to 60:40 over several column volumes. The desired fractions were combined and evaporated to provide the title compound (30 mg) as a yellow gum.

WORKUP

后处理

  1. customthe solution pre-absorbed directly onto silica gel
  2. customThe mixture was purified by chromatography on an Isco Companion
  3. washeluting with ethyl acetate
  4. temperatureheptane, increasing the gradient linearly from 20:80 to 60:40 over several column volumes
  5. customevaporated