反应详情

A solution of 1-(4-Acetyl-phenyl)-ethanone (8.1 g, 5 mmol), in HOAc (50 mL) at 60° C. was treated with bromine (1 eq., 0.26 mL) dropwise over 10 minutes. After 5 more minutes the reaction was cooled, the acetic acid was removed, ethyl acetate (50 mL) was added and then removed to get drive off the remainder of the acetic acid. The crude bromo ketone was then dissolved in ethanol (30 mL) with NaOAc (1.1 g) and thiourea (1 eq., 375 mg) was added. The suspension was stirred at room temperature for 15 hours. The solvents were removed and the resulting mixture was redissolved in 5 ml of 90% DMF, 10% water with 0.1% TFA and purified by reverse phase HPLC to give the product. MS: 219.1 (M+H−).

1. temperatureAfter 5 more minutes the reaction was cooled
2. customthe acetic acid was removed
3. additionethyl acetate (50 mL) was added
4. customremoved
5. customto get
6. additionwas added
7. customThe solvents were removed
8. dissolutionthe resulting mixture was redissolved in 5 ml of 90% DMF
9. custom10% water with 0.1% TFA and purified by reverse phase HPLC
10. customto give the product