Реакция #2045021

Уравнение реакции

2-(4-Aminophenoxy)propionic acid methyl ester

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

triethylamine

triphosgene

→

32

Выход 143.8%

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

Выход 143.8%

Растворители

toluene

Условия реакции

Обработка

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

Методика

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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