Реакция #2045023

Уравнение реакции

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

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

2-(4-Isocyanato-phenoxy)-propionic acid methyl ester

→

34

Выход 61.8%

2-(4-{2-[4-(1-Methoxycarbonyl-ethoxy)-phenylcarbamoyloxy]-ethoxycarbonylamino}-phenoxy)-propionic acid methyl ester

Выход 61.8%

Растворители

toluene

Условия реакции

Обработка

1. 1
   workup.DISTILLATIONToluene was distilled off
2. 2
   workup.ADDITIONwater (50 ml) was added
3. 3
   ФильтрацияThe solids were filtered
4. 4
   Другоеdried
5. 5
   Другоеto give crude 34, which
6. 6
   Другоеwas purified by column chromatography on silica gel

Методика

To 2-[4-(2-Hydroxyethoxycarbonylamino)phenoxy]propionic acid methyl ester 33 (5 g, 17.66 mmol) in toluene (50 ml) was added 2-(4-Isocyanato-phenoxy)-propionic acid methyl ester 32 (3.9 g, 17.64 mmol) at room temperature and heated to 60° C. for 30 hours. Toluene was distilled off and water (50 ml) was added. The solids were filtered and dried to give crude 34, which was purified by column chromatography on silica gel using chloroform as eluant to get pure 34 (5.5 g, 61.8%) as a white powder. M.p: 98-100° C.

Источник