HRID1591127
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
1.58 g (4 millimoles) of N-(4-carbethoxyphenyl)-1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)-2-aminoethanol were stirred with 20 ml of 1N sodium hydrogen phosphite solution and 2 ml (20 millimoles) of formalin solution in 20 ml of dioxane for 1 hour at 60° C. The mixture was then poured onto water and extracted with ether, and the organic phase was washed with 2N sodium hydroxide solution and water, dried over magnesium sulfate and evaporated down. Recrystallization from methanol gave 1.0 g of the title compound, Rf =0.51 (thin layer chromatography, silica gel; 7:1 n-heptane/ethyl acetate).
WORKUP
后处理
- additionThe mixture was then poured onto water
- extractionextracted with ether
- washthe organic phase was washed with 2N sodium hydroxide solution and water
- dry with materialdried over magnesium sulfate
- customevaporated down
- customRecrystallization from methanol