반응 #52976

반응 방정식

(MeO)3B

n-BuLi

1-Bromo-2,6-dichlorobenzene

Water

→

2,6-dichlorobenzeneboronic acid

용매

HOAc

hexane

THF

반응 조건

후처리

1. 1
   온도to warm to room temperature
2. 2
   workup.STIRRINGstirred overnight
3. 3
   workup.STIRRINGthe resulting mixture was stirred for 0.5 h
4. 4
   추출extracted with EtOAc
5. 5
   세척The organic layer was further washed with water and brine
6. 6
   건조dried (MgSO4)
7. 7
   여과filtered
8. 8
   기타evaporated

실험 절차

1-Bromo-2,6-dichlorobenzene (2.00 g) was dissolved in freshly distilled THF (7 mL). This solution was cooled to −78° C. and n-BuLi (8.3 mL of a 1.6M solution in hexane) was added dropwise to the cold solution under N2. The mixture was stirred for 5 min at −78° C. and (MeO)3B (2.2 mL) was added. The resulting mixture was allowed to warm to room temperature and stirred overnight. Water was added and the resulting mixture was stirred for 0.5 h, then acidified with HOAc and extracted with EtOAc. The organic layer was further washed with water and brine, dried (MgSO4) filtered and evaporated to yield 2,6-dichlorobenzeneboronic acid (1.6 g).

출처