Reaktion #725904

Reaktionsgleichung

2-(4-Aminophenoxy)propionic acid methyl ester

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

triethylamine

triphosgene

→

32

Ausbeute 143.8%

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

Ausbeute 143.8%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle