反応 #725899

反応方程式

4-aminophenol

sodium bicarbonate

benzyloxy acetyl chloride

→

26

収率 48.9%

2-Benzyloxy-N-(4-hydroxy-phenyl)-acetamide

収率 48.9%

溶媒

acetone

反応条件

後処理

1. 1
   ろ過The solids were filtered off
2. 2
   workup.ADDITIONcold water (500 ml) was added
3. 3
   抽出Crude 26 was extracted into chloroform
4. 4
   洗浄washed with 5% sodium bicarbonate solution (2×100 ml), water (2×100 ml)
5. 5
   乾燥dried over sodium sulphate
6. 6
   workup.DISTILLATIONdistilled
7. 7
   その他The crude 26 was purified by column chromatography on silica gel

実験手順

To mixture of 4-aminophenol (20 g, 183.2 mmol) and sodium bicarbonate (17 grams, 202 mmol) in acetone (150 ml) at 0° C. was added benzyloxy acetyl chloride (40 g, 216.8 mmol) drop wise, followed by stirring at room temperature for 20 hours. The solids were filtered off, and cold water (500 ml) was added. Crude 26 was extracted into chloroform, washed with 5% sodium bicarbonate solution (2×100 ml), water (2×100 ml), dried over sodium sulphate and distilled. The crude 26 was purified by column chromatography on silica gel using chloroform as eluant to get pure 26 (23 g, 48.9%) as a light orange syrup.

出典