反応 #725904

反応方程式

2-(4-Aminophenoxy)propionic acid methyl ester

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

triethylamine

triphosgene

→

32

収率 143.8%

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

収率 143.8%

溶媒

toluene

反応条件

後処理

1. 1
   温度maintained at this temp
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   ろ過the solids were filtered off
4. 4
   workup.DISTILLATIONthe toluene was distilled off under vacuum
5. 5
   その他to get crude 32, which
6. 6
   workup.DISTILLATIONdistilled

実験手順

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.

出典