反应详情

温度

110 °C

A mixture of azidoacetic acid (5.0 grams, 50 mmol.) and ethyl cyanoformate (15.0 grams, 150 millimoles,) was heated at 110°C. for 8.5 hours. The reaction mixture was cooled; crystalline product separated which was filtered and washed with toluene. The filtrate was concentrated under vacuum, and the remaining oil was cooled and seeded with a crystal of the product to give a second crop. The yield of the title product was 5.1 grams (51 percent, assuming pure starting materials), m.p. (both crops) 144°-147°C. The analysis was as follows:

1. temperatureThe reaction mixture was cooled
2. customcrystalline product separated which
3. filtrationwas filtered
4. washwashed with toluene
5. concentrationThe filtrate was concentrated under vacuum
6. temperaturethe remaining oil was cooled
7. customto give a second crop