HRID409010
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
Benzoyl chloride (1.92 mL, 0.0166 mol) was added to a solution of ((5S,6aR)-2,2,6a-trimethyl-dihydro-5H-furo[3,2-d][1,3]dioxol-5-yl)methanol (from step 8) (2.72 g, 0.0138 mol) in 20 mL of anhydrous pyridine at 0° C. To this mixture 5 mol % of DMAP was added and stirred at room temperature for 3 h. Pyridine was removed under vacuum; the residue was diluted with ethyl acetate and washed with 1N HCl, saturated NaHCO3 and brine. The organic layers were dried over anhydrous Na2SO4, filtered and concentrated. The compound was purified via column chromatography using hexane and ethyl acetate as a gradient mixture to give 4.1 g of the title compound (97% yield).
WORKUP
后处理
- customPyridine was removed under vacuum
- additionthe residue was diluted with ethyl acetate
- washwashed with 1N HCl, saturated NaHCO3 and brine
- dry with materialThe organic layers were dried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe compound was purified via column chromatography