反应 #2200606

反应方程式

Thioformamide

ethyl 2-chloroacetoacetate

magnesium carbonate

→

4-methyl-5-(ethoxycarbonyl)thiazole

溶剂

dioxane

反应条件

后处理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   过滤filtered
3. 3
   其他to remove magnesium carbonate
4. 4
   其他The solvent was evaporated to dryness
5. 5
   洗涤washed successively with 0.5 M NaOH solution (200 mL×2) and saturated brine solution (100 mL)
6. 6
   干燥dried over Na2SO4
7. 7
   过滤It was filtered
8. 8
   其他evaporated

实验过程

Thioformamide (7.5 g, 122.72 mmol), ethyl 2-chloroacetoacetate (16.4 g, 99.52 mmol) and magnesium carbonate (20 g, 237.22 mmoL) were taken dioxane (100 mL) and heated at 110° C. for 4 hrs. The reaction mixture was cooled to room temperature and filtered to remove magnesium carbonate. The solvent was evaporated to dryness and the residue was taken in ether (200 mL) and washed successively with 0.5 M NaOH solution (200 mL×2) and saturated brine solution (100 mL) and dried over Na2SO4. It was filtered and evaporated to give 4-methyl-5-(ethoxycarbonyl)thiazole as an oil which was purified by silica gel column chromatography using hexanes:EtOAc (8:2, v/v) as a eluent; yield: 3.28 g (17%).

来源