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 mixture of (R)-2-methylpropane-2-sulfinamide (2.4326 g, 20.07 mmol) and Cs2CO3 (9.81 g, 30.1 mmol) in DCM (50 mL) was added dropwise a solution of 3-bromobenzaldehyde (4.08 g, 22.08 mmol) in DCM (50 mL) over 10 min and the mixture stirred at ambient temperature for overnight. The reaction mixture was filtered through celite and the filter pad washed with DCM then with EtOAc. Filtrate was dried over MgSO4 and concentrated to give an oil which was purified by silica gel chromatography to give 161A (4.7626 g, 16.53 mmol, 82% yield) as an faint yellow colored oil. 1H NMR (500 MHz, CDCl3) δ 8.55 (s, 1H), 8.05 (t, J=1.8 Hz, 1H), 7.76 (dt, J=7.7, 1.2 Hz, 1H), 7.68-7.65 (m, 1H), 7.41-7.36 (m, 1H), 1.31-1.29 (m, 9H).
WORKUP
后处理
- filtrationThe reaction mixture was filtered through celite
- washthe filter pad washed with DCM
- dry with materialFiltrate was dried over MgSO4
- concentrationconcentrated
- customto give an oil which
- customwas purified by silica gel chromatography