反应详情

温度

50 °C

Concentrated hydrochloric acid was added dropwise to a solution of piperazine (0.124 mol) in water (110 ml) to adjust the pH to 2.8. The solution was then heated to 50° C. 4-Fluorobenzoyl chloride (0.124 mol) was added to the warm solution dropwise while maintaining the pH at 2.8 by the concurrent addition of 40% aqueous sodium acetate solution. After complete addition, a solution of potassium carbonate (47 g) in water (50 ml) was added and the mixture cooled in an ice bath. The cold mixture was extracted with chloroform (5×150 ml). The combined extracts were dried (MgSO4) and evaporated in vacuo affording 22.5 g of a white solid (88% yield). Spectral data are consistent with the assigned structure. This material was used without further purification.

1. temperaturewhile maintaining the pH at 2.8
2. additionAfter complete addition
3. temperaturethe mixture cooled in an ice bath
4. extractionThe cold mixture was extracted with chloroform (5×150 ml)
5. dry with materialThe combined extracts were dried (MgSO4)
6. customevaporated in vacuo