반응 #69620

반응 방정식

magnesium

1-bromo-4,4,4-trifluorobutane

3-pentanone

→

7,7,7-trifluoro-3-ethyl-3-heptanol

수율 76.1%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   기타equipped with a nitrogen feeding pipe, a reflux condenser, a dropping funnel
2. 2
   workup.ADDITIONThe reaction mixture was treated by a conventional method
3. 3
   세척the resulting organic phase was washed with water
4. 4
   건조by drying with anhydrous magnesium sulfate
5. 5
   농축Thereafter, the resultant was concentrated under reduced pressure

실험 절차

1.3 g of magnesium, 10.0 g of 1-bromo-4,4,4-trifluorobutane and 20 g of tetrahydrofuran were added to a four-necked flask equipped with a nitrogen feeding pipe, a reflux condenser, a dropping funnel and a thermometer, and a Grignard reagent was prepared by a conventional method. Then, a mixture containing 5.0 g of 3-pentanone and 4 g of tetrahydrofuran was dropwise added to the obtained Grignard reagent at a temperature of 25 to 35° C. over 30 minutes, followed by stirring at the same temperature for 1 hour. The reaction mixture was treated by a conventional method, and the resulting organic phase was washed with water, followed by drying with anhydrous magnesium sulfate. Thereafter, the resultant was concentrated under reduced pressure, thereby obtaining 7.9 g of 7,7,7-trifluoro-3-ethyl-3-heptanol in the form of a pale yellow oily matter.

출처