反応 #2045023

反応方程式

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

収率 61.8%

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

収率 61.8%

溶媒

toluene

反応条件

後処理

1. 1
   workup.DISTILLATIONToluene was distilled off
2. 2
   workup.ADDITIONwater (50 ml) was added
3. 3
   ろ過The solids were filtered
4. 4
   その他dried
5. 5
   その他to give crude 34, which
6. 6
   その他was purified by column chromatography on silica gel

実験手順

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.

出典