HRID261207
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
1.6 g of sodium borohydride in 20 ml of ethanol are added at 0°-5° to a solution of 10 g of 6-chloro-3a,4,9,9a-tetrahydro-2-methylbenz[f]isoindolin-4-one in 100 ml of ethanol, stirred at room temperature for a further hour, water is added and the mixture evaporated. The residue is taken up in 10% tartaric acid, the aqueous phase extracted with ether, mixed with 2 N caustic soda solution and extracted with ethyl acetate. The ethyl acetate phase is dried over sodium sulphate and evaporated. The residue is crystallised from methylene chloride/pentane to yield 6-chloro-3a,4,9,9a-tetrahydro-2-methylbenz[f]isoindolin-4-ol. M.P. 178°-182°.
WORKUP
后处理
- customthe mixture evaporated
- extractionthe aqueous phase extracted with ether
- additionmixed with 2 N caustic soda solution
- extractionextracted with ethyl acetate
- dry with materialThe ethyl acetate phase is dried over sodium sulphate
- customevaporated
- customThe residue is crystallised from methylene chloride/pentane