HRID273666

反应详情

EQUATION

反应方程式

HRID 273666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Maltol (i.e. 2-methyl-3-hydroxypyran-4-one) 250 g) was dissolved in 25% aqueous methylamine (750 ml) and water (125 ml). The solution was pumped through the CMR (18 ml/min; 160°-2° C.; 900 kPa) and the hot reaction mixture passed directly into acetone (2.5 liters), cooled in an ice water bath. The crystalline product (146 g; 53% yield) was collected by filtration, and washed with acetone (2×250 ml). The corresponding literature method17 involved 6.5 hours at reflux, followed by laborious work up.

WORKUP

后处理

  1. customwas pumped through the CMR (18 ml/min; 160°-2° C.; 900 kPa)
  2. temperaturecooled in an ice water bath
  3. filtrationThe crystalline product (146 g; 53% yield) was collected by filtration
  4. washwashed with acetone (2×250 ml)
  5. temperatureat reflux