HRID273666
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
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
- customwas pumped through the CMR (18 ml/min; 160°-2° C.; 900 kPa)
- temperaturecooled in an ice water bath
- filtrationThe crystalline product (146 g; 53% yield) was collected by filtration
- washwashed with acetone (2×250 ml)
- temperatureat reflux