反应 #1077095

反应方程式

4-methyl-5-(hydroxymethyl)-thiazole

2-chloroacetophenone

Acetonitrile

→

3-(2-Phenyl-2-oxoethyl)-4-methyl-5-(hydroxymethyl)-thiazolium chloride

溶剂

tert-butyl methyl ether

反应条件

后处理

1. 1
   温度the mixture refluxed for another 3 hrs
2. 2
   温度It was cooled to room temperature
3. 3
   workup.WAITthe reaction mixture was left overnight at room temperature
4. 4
   其他The product crystallized
5. 5
   过滤was filtered
6. 6
   洗涤washed well with a mixture of hexanes:EtOAc (1:1
7. 7
   其他v/v) and dried
8. 8
   其他It was recrystallized from a mixture of actonitrile/ethanol/tert-butyl methyl ether

实验过程

The neat reaction of 4-methyl-5-(hydroxymethyl)-thiazole (590 mg, 4.57 mmoL) and 2-chloroacetophenone (710 mg, 4.59 mmoL) was heated at 110° C. The mixture solidified within 15 minutes. Acetonitrile (10 mL) was added and the mixture refluxed for another 3 hrs. It was cooled to room temperature and tert-butyl methyl ether (5 mL) was added and the reaction mixture was left overnight at room temperature. The product crystallized was filtered and washed well with a mixture of hexanes:EtOAc (1:1, v/v) and dried. It was recrystallized from a mixture of actonitrile/ethanol/tert-butyl methyl ether; yield 130 mg (10%); mp. 240-242° C. (dec.).

来源