반응 #725895

반응 방정식

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

반응 조건

후처리

1. 1
   기타at 10° C.
2. 2
   기타for 1 hour
3. 3
   온도refluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (1.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   추출Crude 21 was extracted into chloroform
7. 7
   세척washed with 5% NaHCO3 solution in water
8. 8
   건조dried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

실험 절차

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.

출처