反应详情

A mixture of 67.0 g (0.28 mol) of ethyl 5,5-dichloro-2-isopropyl-4-pentenoate, 77.35 g (0.56 mol) of anhydrous potassium carbonate, 2128 ml of methanol, and 708 ml of water was refluxed 4 days under nitrogen. The reaction mixture was then cooled to room temperature and about two-thirds of the solvent removed on the rotary evaporator. The residue was taken up in three times its volume of water, extracted twice with ether, and acidified with conc. HCl. The acidified reaction mixture was extracted into ether, the ether solution washed with water, dried (MgSO4), and removed. The residue was vacuum distilled to give 52.5 g (89% yield) of 5,5-dichloro-2-isopropyl-4-pentenoic acid, b.p. 91°-96° C./0.30 mm.

1. temperaturewas refluxed 4 days under nitrogen
2. customremoved on the rotary evaporator
3. extractionextracted twice with ether
4. customThe acidified reaction mixture
5. extractionwas extracted into ether
6. washthe ether solution washed with water
7. dry with materialdried (MgSO4)
8. customremoved
9. distillationdistilled