反应详情

A mixture containing 2-bromocinnamic acid (250 mg, 1.10 mmol), the product of step 1 (271 mg, 1.1 equiv.), Pd(OAc)2 (8 mg, 0.03 equiv.), LiCl (47 mg, 1 equiv.), LiOAc (280 mg, 2.5 equiv.) and Bu4NCl (611 mg, 2 equiv.) in DMF (2 ml) was degassed and heated to 100 C. o.n. 0.5 N HCl was then added and the product was extracted in EtOAc, washed with 0.5 N HCl, dried over Na2SO4 and concentrated to dryness. Recrystallization from ether:hexane afforded the title product as a white solid. Yield: 251 mg, 62%.

1. temperatureheated to 100 C
2. extractionthe product was extracted in EtOAc
3. washwashed with 0.5 N HCl
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness
6. customRecrystallization from ether