تفاعل #725901

معادلة التفاعل

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

triethylamine

triphosgene

→

28

المردود 159.1%

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

المردود 159.1%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةLater the reaction mixture was heated to 75° C. over a period of one hour
2. 2
   درجة الحرارةmaintained at this temperature for 26 hours
3. 3
   درجة الحرارةThe reaction mixture was then cooled to room temperature
4. 4
   ترشيحthe solids were filtered off
5. 5
   workup.DISTILLATIONthe toluene was distilled off under vacuum
6. 6
   أخرىto get crude 28, which
7. 7
   workup.DISTILLATIONdistilled

الإجراء التجريبي

To a mixture of (4-Amino-phenoxy)-acetic acid methyl ester 15 (15 g, 82.87 mmol) and triethylamine (16.77 g, 165.73 mmol) in toluene (225 ml) under nitrogen atm. at 0° C. was added triphosgene (9 g, 30.33 mmol) in one lot. The reaction was exothermic and the temperature raised to 25° C. Later the reaction mixture was heated to 75° C. over a period of one hour and maintained at this temperature for 26 hours. The reaction mixture was then cooled to room temperature, the solids were filtered off, and the toluene was distilled off under vacuum to get crude 28, which was vacuum distilled to get pure 28 (10 g, 58.3%) as a white powder. M.p: 50-53° C.

المصدر