HRID2215079
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 a solution of ester 2-2 (560 mg) in ethanol (5 mL) at 0° C. was added NaBH4 (38 mg) and the mixture was stirred at the temperature for 1 h and quenched with half saturated NaCl. The mixture was concentrated in vacuo to remove the ethanol and the residue was extracted with ethyl acetate (3×). The organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford the desired alcohol 2-3 (480 mg). 1H NMR (400 MHz, acetone-d6): δ 4.33 (t, 1H), 4.20–4.12 (m, 2H), 3.96 (m, 1H), 3.79 (m, 1H), 3.65 (m, 1H), 3.40 (m, 1H), 3.17 (m, 1H), 2.47 (t, 2H), 1.70–1.35 (m, 8H).
WORKUP
后处理
- customquenched with half saturated NaCl
- concentrationThe mixture was concentrated in vacuo
- customto remove the ethanol
- extractionthe residue was extracted with ethyl acetate (3×)
- washThe organic layers were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo