تفاعل #2200606

معادلة التفاعل

Thioformamide

ethyl 2-chloroacetoacetate

magnesium carbonate

→

4-methyl-5-(ethoxycarbonyl)thiazole

المذيبات

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was cooled to room temperature
2. 2
   ترشيحfiltered
3. 3
   أخرىto remove magnesium carbonate
4. 4
   أخرىThe solvent was evaporated to dryness
5. 5
   غسيلwashed successively with 0.5 M NaOH solution (200 mL×2) and saturated brine solution (100 mL)
6. 6
   تجفيفdried over Na2SO4
7. 7
   ترشيحIt was filtered
8. 8
   أخرىevaporated

الإجراء التجريبي

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%).

المصدر