반응 #833549

반응 방정식

Bromoacetylbromide

6-nitroveratrylalcohol

Et3N

CH2Cl2

→

4.5-dimethoxy-2-nitrobenzyl 2-bromoacetate

수율 55.1%

용매

CHCl3

반응 조건

후처리

1. 1
   세척the mixture was washed with HCl (1 M, 2×10 ml), NaHCO3 (sat., 10 ml) and water (10 ml)
2. 2
   건조Organic phase was dried over Na2SO4
3. 3
   기타evaporated
4. 4
   기타purified by chromatography (Si-gel, CH2Cl2)

실험 절차

Bromoacetylbromide (0.19 ml, 2.2 mmol) was slowly added to the solution of 6-nitroveratrylalcohol (0.43 g, 2 mmol), Et3N (0.56 ml, 4 mmol) and DMAP (24 mg, 0.2 mmol) in CHCl3 (5 ml). After stirring at room temperature for five hours, CH2Cl2 (20 ml) was added and the mixture was washed with HCl (1 M, 2×10 ml), NaHCO3 (sat., 10 ml) and water (10 ml). Organic phase was dried over Na2SO4, evaporated and purified by chromatography (Si-gel, CH2Cl2) to yield 4.5-dimethoxy-2-nitrobenzyl 2-bromoacetate (368 mg, 55%).

출처