HRID927156

反应详情

EQUATION

反应方程式

HRID 927156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 5,6-bis(benzyloxy)-N-(cyclopropylmethyl)-N-methylpyridazin-3-amine (Intermediate 46; 2.44 mmol) and palladium on carbon (10% wt loading, dry basis; 0.259 g, 0.244 mmol) in ethyl acetate (10 ml) was stirred under a hydrogen atmosphere for 2 hours. The reaction mixture was filtered through a diatomaceous earth cartridge commercially sold under the trade mark ‘Celite’, eluting with ethyl acetate, tetrahydrofuran and methanol. The filtrate was concentrated in vacuo to afford a brown solid, which was triturated from ethyl acetate to give the title compound as a pale brown solid (27.9 mg, 38%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a diatomaceous earth cartridge
  2. washeluting with ethyl acetate, tetrahydrofuran and methanol
  3. concentrationThe filtrate was concentrated in vacuo
  4. customto afford a brown solid, which
  5. customwas triturated from ethyl acetate