反应 #2045005

反应方程式

(4-Aminophenoxy)acetic acid HCl

(4-Amino-phenoxy)acetic acid HCl

HCl

methanol

→

15

收率 58.5%

(4-Amino-phenoxy)-acetic acid methyl ester

收率 58.5%

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 10 hours
4. 4
   workup.DISTILLATIONMethanol (3.5 liters) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   过滤Crude 15 was filtered
7. 7
   其他dried
8. 8
   其他recrystallised from a mixture of chloroform:hexane (1:5)

实验过程

To a mixture of (4-Aminophenoxy)acetic acid HCl 14 (250 g, 1.228 mol), in methanol (5 L) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 10 hours. Methanol (3.5 liters) was distilled off, ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 15 was filtered, dried and recrystallised from a mixture of chloroform:hexane (1:5) to give pure 15 (130 g, 58.5%) as a light brown powder. The melting point was found to be 65-66.8° C.

来源