反应 #2045022

反应方程式

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

ethylene glycol

→

33

收率 50.8%

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

收率 50.8%

溶剂

Water

反应条件

后处理

1. 1
   其他rose to 58° C
2. 2
   温度to cool
3. 3
   萃取crude 33 was extracted into chloroform
4. 4
   洗涤washed with water (2×50 ml)
5. 5
   干燥dried over sodium sulphate
6. 6
   workup.DISTILLATIONdistilled
7. 7
   其他Crude 33 was purified by column chromatography on silica gel

实验过程

2-(4-Isocyanato-phenoxy)-propionic acid methyl ester 32 (20 g, 90.49 mmol) was added to ethylene glycol (40 ml) at room temperature. The reaction was exothermic and the temperature rose to 58° C. The mixture was allowed to cool and later stirred at room temperature for 16 hours. Water (150 ml) was added and crude 33 was extracted into chloroform, washed with water (2×50 ml), dried over sodium sulphate and distilled. Crude 33 was purified by column chromatography on silica gel using chloroform as eluant to get pure 33 (13 gr, 50.76%) as a syrup which crystallized in 48 hours as a white powder. M.p: 90.5-92.8° C.

来源