反应 #2045011

反应方程式

6-(4-Amino-phenoxy)-hexanoic acid hydrochloride

6-(4-Amino-phenoxy)-hexanoic acid Hydrochloride

methanol

HCl

→

21

6-(4-Amino-phenoxy)-hexanoic acid methyl ester

反应条件

后处理

1. 1
   其他at 10° C.
2. 2
   其他for 1 hour
3. 3
   温度refluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (1.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   萃取Crude 21 was extracted into chloroform
7. 7
   洗涤washed with 5% NaHCO3 solution in water
8. 8
   干燥dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

实验过程

To a mixture of 6-(4-Amino-phenoxy)-hexanoic acid hydrochloride 20 (150 grams, 578 mmol) in methanol (3 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 48 hours. Methanol (1.5 liter) was distilled off, ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 21 was extracted into chloroform, washed with 5% NaHCO3 solution in water, dried over Na2SO4 and distilled to give 21 (60 g, 43.8) as a thick brown syrup. The structure was confirmed with NMR.

来源