反应详情

温度

0 °C

To a suspension of sodium hydride (0.724 g, 60% suspension in oil) in N,N-dimethyl formamide (50 mL) was added pyrrole 2-carboxaldehyde (1.7 g, 18.1 mmol) and the reaction mixture was stirred for 30 minutes. It was then cooled to 0° C. and 4,5-dimethoxy-2-nitrobenzyl bromide (5.0 g, 1 equiv) was added dropwise over 20 minutes. After the addition, the reaction mixture was stirred at room temperature for 3 hours. It was then diluted with ethyl acetate (450 mL), washed with water, dried over anhydrous magnesium sulfate, filtered and evaporated to dryness. The crude product was triturated with water, filtered and washed with water. This material was dried over anhydrous potassium carbonate in vacuo to provide the title compound as a yellow crystalline solid (4.97 g), m.p. 109–112° C., which was used in the next step.

1. additionAfter the addition
2. stirringthe reaction mixture was stirred at room temperature for 3 hours
3. washwashed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customevaporated to dryness
7. customThe crude product was triturated with water
8. filtrationfiltered
9. washwashed with water
10. dry with materialThis material was dried over anhydrous potassium carbonate in vacuo