HRID232548
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 8-t-butyl-3-(p-toluenesulfonyloxy)-1-oxaspiro-(4,5)decane (18.3 g, 50 mmol) and sodium cyanide (4.9 g, 100 mmol) in dry DMF (75 ml) was heated to 100° C. for 6 hours. Light petroleum/ethylacetate 4:1 (50 ml) was added and the mixture was filtrated from insoluble material. The filtrate was then evaporated in vacuo and the resulting residue was taken up in toluene (100 ml). It was washed with water, dried (MgSO4) and evaporated in vacuo to yield a brownish oil (11.0 g) which was Kugelrohr distilled (120°-125° C., 0.015 mbar) to furnish the product as colourless crystals (8.94 g, m.p. 35°-40° C.).
WORKUP
后处理
- filtrationthe mixture was filtrated from insoluble material
- customThe filtrate was then evaporated in vacuo
- washIt was washed with water
- dry with materialdried (MgSO4)
- customevaporated in vacuo