HRID379587
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
To a solution of 5-[(3-hydroxypropyl)thio]-3-methyl-1-(2-methylpropyl)-6-[(pyridin-3-yl)carbonyl]thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.35 g, Example 37) in dry ethanol (40 ml) at 0° C. was added sodium borohydride (0.03 g). The reaction was allowed to warm to room temperature and stirred for 2 hours. The solution was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by normal-phase HPLC eluting with a gradient of 0-5% ethanol in dichloromethane to give the title compound as a white foam. (0.27 g).
WORKUP
后处理
- concentrationThe solution was concentrated under reduced pressure
- customThe residue was partitioned between ethyl acetate and water
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by normal-phase HPLC
- washeluting with a gradient of 0-5% ethanol in dichloromethane