تفاعل #2045011

معادلة التفاعل

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

ظروف التفاعل

المعالجة

1. 1
   أخرىat 10° C.
2. 2
   أخرىfor 1 hour
3. 3
   درجة الحرارةrefluxed for 48 hours
4. 4
   workup.DISTILLATIONMethanol (1.5 liter) was distilled off
5. 5
   workup.ADDITIONice water (1 liter) was added
6. 6
   استخلاصCrude 21 was extracted into chloroform
7. 7
   غسيلwashed with 5% NaHCO3 solution in water
8. 8
   تجفيفdried over Na2SO4
9. 9
   workup.DISTILLATIONdistilled

الإجراء التجريبي

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.

المصدر