반응 #725904

반응 방정식

2-(4-Aminophenoxy)propionic acid methyl ester

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

triethylamine

triphosgene

→

32

수율 143.8%

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

수율 143.8%

용매

toluene

반응 조건

후처리

1. 1
   온도maintained at this temp
2. 2
   온도The reaction mixture was cooled to room temperature
3. 3
   여과the solids were filtered off
4. 4
   workup.DISTILLATIONthe toluene was distilled off under vacuum
5. 5
   기타to get crude 32, which
6. 6
   workup.DISTILLATIONdistilled

실험 절차

To a mixture of 2-(4-Aminophenoxy)propionic acid methyl ester 18 (15 grams, 76.9 mmol) and triethylamine (15.6 g, 154.16 mmol) in toluene (210 ml) under nitrogen atm. was added triphosgene (8.4 g, 28.3 mmol) in one lot. Later the reaction mixture was heated to 75° C. over a period of one hour and maintained at this temp. for 26 hours. The reaction mixture was cooled to room temperature, the solids were filtered off, and the toluene was distilled off under vacuum to get crude 32, which was vacuum distilled to get pure 32 (9 g, 52.9%) as a light yellow syrup.

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