反応 #725903

反応方程式

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

(4-Isocyanato-phenoxy)-acetic acid methyl ester

→

30

収率 56.5%

{4-[2-(4-Methoxycarbonylmethoxy-phenylcarbamoyloxy)-ethoxycarbonylamino]-phenoxy}-acetic acid methyl ester

収率 56.5%

溶媒

toluene

反応条件

後処理

1. 1
   workup.DISTILLATIONToluene was distilled off
2. 2
   workup.ADDITIONwater (10 ml) was added
3. 3
   抽出Crude 30 was extracted into chloroform
4. 4
   乾燥dried over sodium sulphate
5. 5
   workup.DISTILLATIONdistilled
6. 6
   その他purified by column chromatography on silica gel

実験手順

To [4-(2-Hydroxy-ethoxycarbonylamino)-phenoxy]-acetic acid methyl ester 29 (1 g, 3.72 mmol) in toluene (10 ml) was added (4-Isocyanato-phenoxy)-acetic acid methyl ester 28 (0.8 g, 3.8 mmol) at room temperature and heated to 50° C. for 20 hours. Toluene was distilled off and water (10 ml) was added. Crude 30 was extracted into chloroform, dried over sodium sulphate, distilled and purified by column chromatography on silica gel using chloroform as eluant to get pure 30 (1 g, 56.5%) as a white fluffy powder.

出典