反応 #833549

反応方程式

Bromoacetylbromide

6-nitroveratrylalcohol

Et3N

CH2Cl2

→

4.5-dimethoxy-2-nitrobenzyl 2-bromoacetate

収率 55.1%

溶媒

CHCl3

反応条件

後処理

1. 1
   洗浄the mixture was washed with HCl (1 M, 2×10 ml), NaHCO3 (sat., 10 ml) and water (10 ml)
2. 2
   乾燥Organic phase was dried over Na2SO4
3. 3
   その他evaporated
4. 4
   その他purified by chromatography (Si-gel, CH2Cl2)

実験手順

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%).

出典