HRID1689436
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 tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate (2 g) in DMF (20 mL) was treated with potassium cyanide (0.672 g) and the resultant mixture stirred at 20° C. for 4 days. The mixture was partitioned between ethyl acetate and brine, the organic layer was washed twice with brine, dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography using 60% ethyl acetate in isohexane as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 1.18 g.
WORKUP
后处理
- customThe mixture was partitioned between ethyl acetate and brine
- washthe organic layer was washed twice with brine
- dry with materialdried over sodium sulphate
- filtrationfiltered
- customthe solvent evaporated under reduced pressure
- customThe crude product was purified by flash silica chromatography
- customPure fractions were evaporated to dryness