반응 #2358449

반응 방정식

hydrochloric acid

methyl magnesium bromide diethyl ether

2,3,4,6-tetrafluorobenzoic acid

water

→

3,4,6-trifluoro-2-methylbenzoic acid

수율 92.0%

용매

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONAfter completion of dropwise addition
2. 2
   온도the reaction mixture was heated to room temperature
3. 3
   추출The reaction mixture was extracted with ethyl acetate
4. 4
   기타separated into liquids
5. 5
   기타The organic layer was separated
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   농축concentrated

실험 절차

200 mg of 2,3,4,6-tetrafluorobenzoic acid was dissolved in 10 ml of diethyl ether and cooled to −10° C. in an argon atmosphere. Then 1.72 ml of a methyl magnesium bromide-diethyl ether solution (3 moles/liter) was added dropwise. After completion of dropwise addition, the reaction mixture was heated to room temperature and stirred at room temperature for 17 hours. The reaction mixture was added to about 50 ml of cold water and adjusted to pH 1 with concentrated hydrochloric acid. The reaction mixture was extracted with ethyl acetate and separated into liquids. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated to give 181 mg of 3,4,6-trifluoro-2-methylbenzoic acid (yield: 92%).

출처