HRID42085
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 solution of 3,3:17,17-bis(ethylendioxy)-6-methyleneandrostane (1.05 g) and pTSA.H2O (2.46 g) in acetone (105 mL) was stirred at room temperature for 3 h. The solution was neutralized by addition of 5% aqueous NaHCO3 and acetone was evaporated. The aqueous suspension was extracted with CH2Cl2 (3×). The combined organic extracts were washed with H2O, dried over Na2SO4 and evaporated to dryness to give the title compound II-ac in 87% yield. 1H-NMR (300 MHz, acetone-d6, ppm from TMS): δ 4.85 (1H, m), 4.50 (1H, m), 2.63-1.02 (20H, m), 0.92 (3H, s), 0.86 (3H, s).
WORKUP
后处理
- customwas evaporated
- extractionThe aqueous suspension was extracted with CH2Cl2 (3×)
- washThe combined organic extracts were washed with H2O
- dry with materialdried over Na2SO4
- customevaporated to dryness