HRID628668
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
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
To a solution of 6,7-dihydroquinolin-8(5H)-one (2.0 g, 13.6 mmol) in ethanol (15 mL) was added concentrated acetic acid (5 drops), tert-butyl 4-aminobutylcarbamate (2.7 g, 14.3 mmol) and 4 Å molecular sieves. The reaction mixture was heated at 150° C. in microwave reactor for 10 min. The mixture was cooled to room temperature and NaBH4 (0.8 g, 20.4 mmol) was added all at once. The crude reaction mixture was absorbed onto silica gel and the product purified by silica gel chromatography (0% to 10% methanol/CH2Cl2) to afford the desired product: ESI+ MS: m/z (rel intensity) 320.2 (100, [M+H]+).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- customThe crude reaction mixture
- customwas absorbed onto silica gel
- customthe product purified by silica gel chromatography (0% to 10% methanol/CH2Cl2)