반응 #2045005

반응 방정식

(4-Aminophenoxy)acetic acid HCl

(4-Amino-phenoxy)acetic acid HCl

HCl

methanol

→

15

수율 58.5%

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

수율 58.5%

반응 조건

후처리

1. 1
   기타at 10° C.
2. 2
   기타for 1 hour
3. 3
   온도refluxed for 10 hours
4. 4
   workup.DISTILLATIONMethanol (3.5 liters) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   여과Crude 15 was filtered
7. 7
   기타dried
8. 8
   기타recrystallised from a mixture of chloroform:hexane (1:5)

실험 절차

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.

출처