반응 #1876813

반응 방정식

Compound ( c )

2-bromo-5-ethoxybenzotrifluoride

butyllithium hexane

hydrochloric acid

Triisopropyl borate

→

Compound ( d )

수율 89.1%

4-ethoxy-2-trifluoromethylphenylboric Acid

수율 89.1%

용매

tetrahydrofuran

THF

반응 조건

후처리

1. 1
   workup.ADDITIONwas then slowly added dropwise at −78° C.
2. 2
   workup.STIRRINGthe mixture was stirred at the same temperature for 1 hour
3. 3
   온도The temperature was increased to room temperature
4. 4
   온도cooling temperature
5. 5
   추출the aqueous layer was extracted three times with ether
6. 6
   세척washed with water
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

Compound (c) (10.0 g) dissolved in tetrahydrofuran (THF) (40 mL) was cooled to −78° C., a 1.6 M butyllithium/hexane solution (30 mL) was slowly added dropwise and the mixture was stirred at the same temperature for 2 hours. Triisopropyl borate (14.0 g) dissolved in THF (20 mL) was then slowly added dropwise at −78° C., and the mixture was stirred at the same temperature for 1 hour. The temperature was increased to room temperature and the final solution was stirred. After adding 3 M hydrochloric acid (200 mL) dropwise at ice-cooling temperature, the aqueous layer was extracted three times with ether. The organic layers were combined, washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 8.28 g of Compound (d).

출처