反応 #2045035

反応方程式

2-(4-Nitro-phenoxy)-propionic acid

ethylene glycol

HCl

→

48

収率 56.8%

2-(4-Nitro-phenoxy)-propionic acid 2-hydroxy-ethyl ester

収率 56.8%

溶媒

water

反応条件

後処理

1. 1
   その他for 1½ hours
2. 2
   その他During HCl gas bubbling the temp
3. 3
   その他rose to 60° C
4. 4
   その他The crude reaction mass
5. 5
   抽出Crude 48 was extracted into chloroform
6. 6
   乾燥dried over Na2SO4
7. 7
   workup.DISTILLATIONdistilled
8. 8
   その他purified by column chromatography on silica gel

実験手順

To a mixture of 2-(4-Nitro-phenoxy)-propionic acid 47 (45 g, 213 mol) and ethylene glycol (135 ml) was passed dry HCl gas for 1½ hours. During HCl gas bubbling the temp. rose to 60° C. The crude reaction mass was poured onto cold water (600 ml). Crude 48 was extracted into chloroform, dried over Na2SO4, distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 48 (28 g, 56.8%) as a syrup.

出典