تفاعل #2045024

معادلة التفاعل

6-(4-amino-phenoxy)hexanoic acid methyl ester

6-(4-Amino-phenoxy)-hexanoic acid methyl ester

triethylamine

triphosgene

→

36

المردود 72.3%

6-(4-Isocyanato-phenoxy)-hexanoic acid methyl ester

المردود 72.3%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىrose to 60° C
2. 2
   درجة الحرارةmaintained at this temperature for 26 hours
3. 3
   درجة الحرارةThe reaction mixture was cooled to room temperature
4. 4
   ترشيحthe solids were filtered
5. 5
   workup.DISTILLATIONthe toluene was distilled off under vacuum
6. 6
   أخرىto get crude 36, which
7. 7
   workup.DISTILLATIONdistilled

الإجراء التجريبي

To a mixture of 6-(4-amino-phenoxy)hexanoic acid methyl ester 21 (26 grams, 109.7 mmol) and triethylamine (29.2 g, 288.56 mmol) in toluene (390 ml) under nitrogen atm. was added triphosgene (15.6 grams, 52.56 mmol) in one lot. The reaction was exothermic and the internal temperature rose to 60° 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 cooled to room temperature, the solids were filtered, and the toluene was distilled off under vacuum to get crude 36, which was vacuum distilled to get pure 36 (10 g, 34.7%). M.p: 47-50° C.

المصدر