تفاعل #2045022

معادلة التفاعل

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

ethylene glycol

→

33

المردود 50.8%

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

المردود 50.8%

المذيبات

Water

ظروف التفاعل

المعالجة

1. 1
   أخرىrose to 58° C
2. 2
   درجة الحرارةto cool
3. 3
   استخلاصcrude 33 was extracted into chloroform
4. 4
   غسيلwashed with water (2×50 ml)
5. 5
   تجفيفdried over sodium sulphate
6. 6
   workup.DISTILLATIONdistilled
7. 7
   أخرىCrude 33 was purified by column chromatography on silica gel

الإجراء التجريبي

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.

المصدر