反应详情

温度

75 °C

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.

1. temperaturemaintained at this temp
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationthe solids were filtered off
4. distillationthe toluene was distilled off under vacuum
5. customto get crude 32, which
6. distillationdistilled