HRID14988
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
- 80 °C
PROCEDURE
实验过程
2.0 g of ethyl 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionate are suspended in 100 ml of methanol, and 32.1 ml of a 2M NaOH solution are added. The reaction mixture is stirred at 80° C. for one hour. The methanol is removed under reduced pressure and the reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid. The mixture is extracted three times with in each case 100 ml of ethyl acetate. The combined organic phases are dried over MgSO4 and then concentrated under reduced pressure. This gives 1.85 g of 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionic acid as a solid.
WORKUP
后处理
- customThe methanol is removed under reduced pressure
- additionthe reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid
- extractionThe mixture is extracted three times with in each case 100 ml of ethyl acetate
- dry with materialThe combined organic phases are dried over MgSO4
- concentrationconcentrated under reduced pressure