HRID1939644

反应详情

EQUATION

反应方程式

HRID 1939644 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A stirred suspension of glycine (18.77 g, 0.25 mol) in methanol (80 ml) and water (4.5 ml) was cooled to 0° C. and adjusted to pH 9.6 by adding 30 percent strength sodium hydroxide solution. Methyl pentanimidate (67.12 g of a 42.9 percent strength solution in toluene=0.25 mol) was added to this suspension over the course of 7 minutes. The reaction mixture was stirred for 5 hours at room temperature. Methanol and water were then distilled off at a reduced pressure of 30 mbar to 150 mbar. In total, 250 ml of toluene was added during this distillation. The mixture was then filtered, and the filter cake washed with toluene (75 ml) and dried. The yield of the title compound was 39.61 g (purity approximately 90 percent by H-NMR), 90 percent based on glycine.

WORKUP

后处理

  1. distillationMethanol and water were then distilled off at a reduced pressure of 30 mbar to 150 mbar
  2. additionIn total, 250 ml of toluene was added during this distillation
  3. filtrationThe mixture was then filtered
  4. washthe filter cake washed with toluene (75 ml)
  5. customdried