反应详情

温度

120 °C

2-Methyl-pentan-3-ol (prepared as above in EXAMPLE I) (153 g), 2-methyl-but-2-enoic acid (100 g), toluene (200 mL), and PTSA (8 g) were charged into to 2-L reaction flask fitted with a Dean-Stark trap. The reaction mixture was heated to reflux at about 120° C. Water was removed. The reaction mixture was aged at reflux for about 13-14 hours till GC analysis showed completion of the reaction. The resulting reaction mixture was washed sequentially with sodium bicarbonate and brine, and further purified by fractional distillation to provide 2-methyl-but-2-enoic acid 1-ethyl-2-methyl-propyl ester (81 g) with a boiling point of 91° C. at 1.1 mmHg.

1. customfitted with a Dean-Stark trap
2. temperatureThe reaction mixture was heated
3. customWater was removed
4. temperatureat reflux for about 13-14 hours till GC analysis
5. customcompletion of the reaction
6. customThe resulting reaction mixture
7. washwas washed sequentially with sodium bicarbonate and brine
8. distillationfurther purified by fractional distillation