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
2.9 g (7.4 mmol) of methyl 2-hydroxy-4-[3-oxo-3-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)-1-propynyl]benzoate and 100 ml of a methanol/THF (50/50) mixture were introduced into a round-bottomed flask and 140 mg (3.7 mmol) of sodium borohydride were added in small amounts. The reaction mixture was stirred at room temperature for 2 hours, poured into water and extracted with ethyl ether. The organic phase was separated by settling, dried over magnesium sulfate and evaporated. The residue obtained was purified by chromatography on a silica column eluted with a mixture of dichloromethane and hexane (50/50). After evaporation of the solvents, 1.6 g (55%) of the expected compound, with a melting point of 92°-93° C., was recovered.
WORKUP
后处理
- extractionextracted with ethyl ether
- customThe organic phase was separated
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe residue obtained
- customwas purified by chromatography on a silica column
- washeluted with a mixture of dichloromethane and hexane (50/50)
- customAfter evaporation of the solvents, 1.6 g (55%) of the expected compound
- customwith a melting point of 92°-93° C., was recovered