HRID48238
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of the product from Example 92 (0.67 g, 1.7 mmol) in 20 ml tetrahydrofuran was treated with Raney nickel (0.1 g) and stirred under a hydrogen atmosphere (1 atm) for 48 hours. The Raney nickel was removed with a magnet and washed with methanol. The remaining solid was collected by filtration, washed with methanol and then dissolved in 2 N HCl and filtered. The filtrate was neutralized with saturated sodium bicarbonate and the precipitate collected by filtration and dried to give the title compound (0.30 g, 57% yield) mp>300° C.
WORKUP
后处理
- customThe Raney nickel was removed with a magnet
- washwashed with methanol
- filtrationThe remaining solid was collected by filtration
- washwashed with methanol
- dissolutiondissolved in 2 N HCl
- filtrationfiltered
- filtrationthe precipitate collected by filtration
- customdried