반응 #43468

반응 방정식

compound 7B

2-Chloro-4-(hydroxymethyl)-3-methylbenzonitrile

PBr3

→

title compound

수율 28.3%

4-(Bromomethyl)-2-chloro-3-methylbenzonitrile

수율 28.3%

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타The reaction was slowly quenched with saturated NaHCO3 solution at −15° C
2. 2
   기타The organic layer was separated
3. 3
   건조dried over MgSO4
4. 4
   농축concentrated
5. 5
   기타Purification by silica gel chromatography (0-10% EtOAc in hexanes)

실험 절차

To a solution of compound 7B (700 mg, 3.9 mmol) in CH2Cl2 (15 mL) was added PBr3 (5.8 mL, 5.8 mmol, 1N in CH2Cl2) at −15° C., and stirred at −15° C. for 3 hr. The reaction was slowly quenched with saturated NaHCO3 solution at −15° C. The organic layer was separated, dried over MgSO4, and concentrated. Purification by silica gel chromatography (0-10% EtOAc in hexanes) provide the title compound (270 mg) as a white powder.

출처