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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
2-methyl-1-phenylpropan-2-yl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate (15.38 g) prepared in Example 19 was dissolved in tetrahydrofuran (80 ml) and a 0.1M hydrochloric acid aqueous solution (19.21 ml) was added thereto, followed by stirring for 24 hours while heating to 40° C. The reaction liquid was cooled to room temperature and a 0.5M sodium hydroxide aqueous solution (81 ml) was added thereto over 5 minutes, followed by stirring for 4 hours. Ethyl acetate (250 ml) and purified water (250 ml) were added to the reaction liquid, and the organic layer was separated, washed with saturated sodium chloride (150 ml), dried over anhydrous sodium sulfate, filtered, and then concentrated under reduced pressure to give (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl](3R,5S)-3,5-dihydroxyhept-6-enoic acid sodium salt.
WORKUP
后处理
- customThe reaction liquid
- temperaturewas cooled to room temperature
- waitover 5 minutes
- stirringby stirring for 4 hours
- customEthyl acetate (250 ml) and purified water (250 ml)
- additionwere added to the reaction liquid
- customthe organic layer was separated
- washwashed with saturated sodium chloride (150 ml)
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure