HRID1004

反应详情

EQUATION

反应方程式

HRID 1004 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6.5 g of 4-[O-benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine in 70 ml of methanol are hydrogenated using 2 g of Raney nickel at normal pressure until absorption of hydrogen is complete. After filtering, the filtrate is concentrated and the product is dissolved in diisopropyl ether. Crystallization takes place on addition of hexane. 4.3 g=90%; m.p.: 45° C.

WORKUP

后处理

  1. customuntil absorption of hydrogen
  2. filtrationAfter filtering
  3. concentrationthe filtrate is concentrated
  4. dissolutionthe product is dissolved in diisopropyl ether
  5. customCrystallization
  6. additionon addition of hexane