反应 #2045008

反应方程式

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

HCl

methanol

→

18

收率 37.2%

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

收率 37.2%

反应条件

后处理

1. 1
   其他at 10° C.
2. 2
   其他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
   萃取Crude 18 was extracted into chloroform
7. 7
   洗涤washed with 5% NaHCO3 solution, water
8. 8
   干燥dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

实验过程

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.

来源