Реакция #2045008

Уравнение реакции

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

HCl

methanol

→

18

Выход 37.2%

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

Выход 37.2%

Условия реакции

Обработка

1. 1
   Другоеat 10° C.
2. 2
   Другоеfor 1 hour
3. 3
   Температураrefluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (2.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   ЭкстракцияCrude 18 was extracted into chloroform
7. 7
   Промывкаwashed with 5% NaHCO3 solution, water
8. 8
   Сушкаdried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

Методика

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.

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