تفاعل #2045008

معادلة التفاعل

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

HCl

methanol

→

18

المردود 37.2%

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

المردود 37.2%

ظروف التفاعل

المعالجة

1. 1
   أخرىat 10° C.
2. 2
   أخرىfor 1 hour
3. 3
   درجة الحرارةrefluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (2.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   استخلاصCrude 18 was extracted into chloroform
7. 7
   غسيلwashed with 5% NaHCO3 solution, water
8. 8
   تجفيفdried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

الإجراء التجريبي

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.

المصدر