반응 #725901

반응 방정식

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

triethylamine

triphosgene

→

28

수율 159.1%

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

수율 159.1%

용매

toluene

반응 조건

후처리

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

실험 절차

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.

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