HRID1675183

反应详情

EQUATION

反应方程式

HRID 1675183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureheated
  2. temperatureto reflux overnight under an atmosphere of nitrogen
  3. customThe solvent was removed in vacuo
  4. customthe resulting orange oil was purified by flash column chromatography on silica gel using
  5. washa gradient elution of 0-7% (MeOH/NH3)/CH2Cl2
  6. customCollection and concentration of the appropriate fractions