反応 #725895

反応方程式

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

反応条件

後処理

1. 1
   その他at 10° C.
2. 2
   その他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
   抽出Crude 21 was extracted into chloroform
7. 7
   洗浄washed with 5% NaHCO3 solution in water
8. 8
   乾燥dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

実験手順

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.

出典