反应详情

A mixture of 3-methyl-but-2-enoic acid (100 g, 1 mol) and SOCl2 (119 g, 1 mol) was heated at reflux for 3 h. The excess SOCl2 was removed under reduced pressure. CH2Cl2 (200 mL) was added followed by the addition of aniline (93 g, 1.0 mol) in Et3N (101 g, 1 mol) at 0° C. The mixture was stirred at room temperature for 1 h and quenched with HCl (5%, 150 mL). The aqueous layer was separated and extracted with CH2Cl2. The combined organic layers were washed with water (2×100 mL) and brine (100 mL), dried over Na2SO4 and concentrated to give 3-methyl-but-2-enoic acid phenylamide (120 g, 80%).

1. temperaturewas heated
2. temperatureat reflux for 3 h
3. customThe excess SOCl2 was removed under reduced pressure
4. additionCH2Cl2 (200 mL) was added
5. customquenched with HCl (5%, 150 mL)
6. customThe aqueous layer was separated
7. extractionextracted with CH2Cl2
8. washThe combined organic layers were washed with water (2×100 mL) and brine (100 mL)
9. dry with materialdried over Na2SO4
10. concentrationconcentrated