HRID393383
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 mixture of 2,2-dimethyl-5-[2-(2-amino-6-chloropurin-9-yl)]ethylidene-1,3-dioxane (0.45 g), 5% palladium on carbon (0.225 g) and triethylamine (0.22 ml) in ethyl acetate (22.5 ml) was hydrogenated at 50° C. for 18 hours at 50 p.s.i. The catalyst was removed by filtration and the filter washed with ethyl acetate. The combined filtrate and wash were concentrated under reduced pressure to give a gum which was purified by silica gel chromatography (eluted with dichloromethane/methanol 99:1 increasing to 97:3) to give the title compound (300 mg, 74% yield).
WORKUP
后处理
- customThe catalyst was removed by filtration
- washthe filter washed with ethyl acetate
- washThe combined filtrate and wash
- concentrationwere concentrated under reduced pressure
- customto give a gum which
- customwas purified by silica gel chromatography (eluted with dichloromethane/methanol 99:1 increasing to 97:3)