HRID574672
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 step B product, 3-d, (25 g, crude) in THF/H2O (1000 mL, VTHF/VH2O=1:1) was added with Na2S2O4 (33.3 g, 191.6 mmol) and stirred at room temperature for 4 h. The reaction mixture was extracted with EA (1000 mL), washed with brine (200 mL), and concentrated in vacuum. The residue was purified by column chromatography to afford the product, 3-e, (7.8 g) as a white solid. 1H NMR (300 MHz, CDCl3): δ 4.42 (s, 2H), 4.63 (s, 2H), 7.33-7.36 (m, 6H). LC-MS (M+H)+ 232.1
WORKUP
后处理
- extractionThe reaction mixture was extracted with EA (1000 mL)
- washwashed with brine (200 mL)
- concentrationconcentrated in vacuum
- customThe residue was purified by column chromatography