反応 #2045005

反応方程式

(4-Aminophenoxy)acetic acid HCl

(4-Amino-phenoxy)acetic acid HCl

HCl

methanol

→

15

収率 58.5%

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

収率 58.5%

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

実験手順

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.

出典