تفاعل #725909

معادلة التفاعل

6-[4-(2-Hydroxyethoxycarbonylamino)phenoxy]hexanoic acid methyl ester

6-[4-(2-Hydroxy-ethoxycarbonylamino)-phenoxy]-hexanoic acid methyl ester

6-(4-Isocyanatophenoxy) hexanoic acid methyl ester

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

→

38

المردود 95.0%

6-(4-{2-[4-(5-Methoxycarbonyl-pentyloxy)-phenylcarbamoyloxy]-ethoxycarbonylamino}-phenoxy)-hexanoic acid methyl ester

المردود 95.0%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONToluene was distilled off
2. 2
   workup.ADDITIONwater (50 ml) was added
3. 3
   ترشيحThe solid was filtered
4. 4
   أخرىdried
5. 5
   أخرىto give crude 38, which
6. 6
   أخرىwas purified by column chromatography on silica gel

الإجراء التجريبي

To a mixture of 6-[4-(2-Hydroxyethoxycarbonylamino)phenoxy]hexanoic acid methyl ester 37 (5 g, 15.38 mmol) in toluene (50 ml) was added 6-(4-Isocyanatophenoxy) hexanoic acid methyl ester 36 (4 g, 15.2 mmol) at room temperature and heated to 60° C. for 2 hours. Toluene was distilled off and water (50 ml) was added. The solid was filtered and dried to give crude 38, which was purified by column chromatography on silica gel using chloroform as eluant to get pure 38 (8.5 g, 94%) as a white powder. M.p: 118-120.5° C.

المصدر