HRID907465
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 containing the ester 18 (21.11 g, 89.4 mmol) and 10 M NaOH (36 ml, 4 equiv) in THF (220 ml), MeOH (110 ml) and water (55 ml) was stirred at reflux for 4 days. Half-saturated NH4Cl (600 ml) and AcOH (25 ml) were then added and the acid 19 was extracted into i-PrOAc. The organics were dried over Na2SO4 and concentrated. Trituration of the residue in ether:hexane 1:3 (200 ml) yielded 18.15 g (91%) of 19 as a white solid.
WORKUP
后处理
- temperatureat reflux for 4 days
- extractionthe acid 19 was extracted into i-PrOAc
- dry with materialThe organics were dried over Na2SO4
- concentrationconcentrated