HRID1675183
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 N1-benzylglycinamide (3.00 g, 14.95 mmol) in MeOH (25 mL) were added acetone (5.50 mL, 74.75 mmol) and triethylamine (1.67 mL, 11.96 mmol). The solution was stirred and heated to reflux overnight under an atmosphere of nitrogen. The solvent was removed in vacuo, and the resulting orange oil was purified by flash column chromatography on silica gel using a gradient elution of 0-7% (MeOH/NH3)/CH2Cl2. Collection and concentration of the appropriate fractions afforded the product as a yellow oil. 1H NMR (400 MHz, CDCl3) δ 7.31-7.27 (m, 5H), 4.44 (s, 2H), 3.55 (s, 2H), 1.26 (s, 6H); ES MS (M+1)=205.
WORKUP
后处理
- temperatureheated
- temperatureto reflux overnight under an atmosphere of nitrogen
- customThe solvent was removed in vacuo
- customthe resulting orange oil was purified by flash column chromatography on silica gel using
- washa gradient elution of 0-7% (MeOH/NH3)/CH2Cl2
- customCollection and concentration of the appropriate fractions