反応 #725892

反応方程式

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

HCl

methanol

→

18

収率 37.2%

2-(4-Amino-phenoxy)-propionic acid methyl ester

収率 37.2%

反応条件

後処理

1. 1
   その他at 10° C.
2. 2
   その他for 1 hour
3. 3
   温度refluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (2.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   抽出Crude 18 was extracted into chloroform
7. 7
   洗浄washed with 5% NaHCO3 solution, water
8. 8
   乾燥dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

実験手順

To a mixture of 2-(4-Amino-phenoxy)-propionic acid 17 (240 g, 1.103 mol), in methanol (4.8 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 48 hours. Methanol (2.5 liter) was distilled off, ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 18 was extracted into chloroform, washed with 5% NaHCO3 solution, water, dried over Na2SO4 and distilled to give 18 (80 g, 37.2%) as a brown syrup. The structure was confirmed with NMR.

出典