反应详情

1.85 g (40 mmols) of formic acid are introduced into a 50 ml two necked flask equipped with an air condenser and a dropping funnel. The flask is cooled on an ice bath and 2 ml of ethylamine are added dropwise. The reaction mixture is allowed to return to ambient temperature and 2.85 g (10 mmols) of 1-(3'-trifluoromethylthio-phenyl)-2-propanone are added. The contents of the flask are heated for 14 hours at 160°-170° C, 2 ml of concentrated hydrochloric acid and 2 ml of water are added, and the mixture is heated for 3 hours at the reflux temperature. A further 2 ml of concentrated hydrochloric acid are added and the mixture is heated again at the reflux temperature for 2 hours. The mixture is allowed to cool, water is added and the product is extracted once with 50 ml of diethyl ether. The aqueous layer is rendered alkaline with sodium hydroxide solution and extracted three times in succession with 50 ml of diethyl ether each time. The combined ether extracts are washed several times with water, dried over sodium sulphate, and filtered. The ether is evaporated from the filtrate in vacuo on a water bath. The 1.4 g of oily residue are dissolved in anhydrous diethyl ether and a solution of hydrogen chloride in diethyl ether is added until precipitation has ended.

1. customequipped with an air condenser and a dropping funnel
2. temperatureThe flask is cooled on an ice bath
3. customto return to ambient temperature
4. temperatureThe contents of the flask are heated for 14 hours at 160°-170° C
5. temperaturethe mixture is heated for 3 hours at the reflux temperature
6. temperaturethe mixture is heated again at the reflux temperature for 2 hours
7. temperatureto cool
8. extractionthe product is extracted once with 50 ml of diethyl ether
9. extractionextracted three times in succession with 50 ml of diethyl ether each time
10. washThe combined ether extracts are washed several times with water
11. dry with materialdried over sodium sulphate
12. filtrationfiltered
13. customThe ether is evaporated from the filtrate in vacuo on a water bath
14. dissolutionThe 1.4 g of oily residue are dissolved in anhydrous diethyl ether
15. additiona solution of hydrogen chloride in diethyl ether is added until precipitation