HRID1648918
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 5.90 g of 1-formyl-3-hydroxy-3-(α-phenyl-2-tolyl)pyrrolidine in 60 ml of dry THF is added dropwise to a suspension of 3 g of LiAlH in 30 ml of dry THF and the mixture is refluxed for 4 hours. After cooling the mixture is separated and the residue extracted with ether. The combined organic solution is dried (Na2SO4) and concentrated to an oil. This oil is dissolved in 100 ml of hexane and after cooling 16 hours the product is isolated by filtration to provide 3-hydroxy-1-methyl-3-(α-phenyl-2-tolyl)pyrrolidine, mp 108°-109° C. Dilution of the mother liquor with 50 ml of hexane gives a second crop of 3-hydroxy-1-methyl-3-(α-phenyl-2-tolyl)pyrrolidine, mp 107°-108° C.
WORKUP
后处理
- temperaturethe mixture is refluxed for 4 hours
- temperatureAfter cooling the mixture
- customis separated
- extractionthe residue extracted with ether
- dry with materialThe combined organic solution is dried (Na2SO4)
- concentrationconcentrated to an oil
- dissolutionThis oil is dissolved in 100 ml of hexane
- temperatureafter cooling 16 hours the product
- customis isolated by filtration