HRID1374198
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 ester 112 (7.26 g, 0.018 mol) in H2O (53 mL) and THF (176 mL) at 0° C. was added a premixed solution of LiOH (37 mL of a 0.8 M solution) and H2O2 (10.57 mL of a 30% solution) and the solution warmed to room temperature. After 2 hours sodium bisulfite (7 g), sodium sulfite (13 g), and water (60 mL) was added and the two layers were separated and the aqueous layer extracted with ether. The combined organic phases were concentrated to an oil that was dissolved in heptane (200 mL). The resultant solid was filtered off and the filtrate dried (MgSO4) and concentrated to afford an oil (4.4 g) that was used without further purification.
WORKUP
后处理
- customthe two layers were separated
- extractionthe aqueous layer extracted with ether
- concentrationThe combined organic phases were concentrated to an oil that
- dissolutionwas dissolved in heptane (200 mL)
- filtrationThe resultant solid was filtered off
- dry with materialthe filtrate dried (MgSO4)
- concentrationconcentrated