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
Sodium borohydride (227 mg, 6.00 mmol) was dissolved in methanol (10 mL) and 5% potassium hydroxide in methanol (4.49 mL, 4.00 mmol) was carefully added. To this solution was added 2-Amino-1-(4-bromo-phenyl)-ethanone hydrochloride (1.0 g, 4.00 mmol) dissolved in methanol (10 mL) and stirring continued for 0.2 hours at room temperature. The mixture was concentrated, and quenched with saturated sodium bicarbonate (10 mL) and extracted with dichloromethane several times. The organics were combined, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The title compound was isolated as a yellow solid (677 mg, 77%). 1H NMR (300 MHz, CDCl3): 7.51-7.47 (d. 2H), 7.27-7.23 (d, 2H), 4.63-4.59 (m, 1H), 3.03 (dd, 1H), 2.76 (dd, 1H)
WORKUP
后处理
- concentrationThe mixture was concentrated
- customquenched with saturated sodium bicarbonate (10 mL)
- extractionextracted with dichloromethane several times
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo