반응 #2045008

반응 방정식

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

HCl

methanol

→

18

수율 37.2%

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

수율 37.2%

반응 조건

후처리

1. 1
   기타at 10° C.
2. 2
   기타for 1 hour
3. 3
   온도refluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (2.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   추출Crude 18 was extracted into chloroform
7. 7
   세척washed with 5% NaHCO3 solution, water
8. 8
   건조dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

실험 절차

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.

출처