反应详情

温度

3.5 °C

To a solution, cooled to 2-5°C. on an ice bath, of 4.4 g (52.36 mmol) of cyanoacetamide in 70 mL of anhydrous DMF are added portionwise 4.19 g (104.72 mmol) of 60% sodium hydride. The mixture is stirred for 15 minutes at 2-5°C., and this suspension is then added rapidly to a solution of 12.35 g (49.87 mmol) of the acid fluoride prepared in step 17.2 in 70 mL of anhydrous DMF, precooled to 2-5°C. The mixture is stirred overnight at room temperature and is then cooled to 2-5°C. on an ice bath, and 2.09 g (52.36 mmol) of 60% sodium hydride are added portionwise. The reaction mixture is stirred for 3 hours at room temperature and then poured into a mixture of ice, 100 mL of water and 150 mL of aqueous 1N HCl. The yellow precipitate formed is isolated by filtration, rinsed with water and then dried in an oven. After triturating in methanol and drying in an oven, 8.84 g of the expected product are finally obtained in the form of a yellow solid. Yield=57%.

1. customprecooled to 2-5°C
2. stirringThe mixture is stirred overnight at room temperature
3. temperatureis then cooled to 2-5°C. on an ice bath
4. stirringThe reaction mixture is stirred for 3 hours at room temperature
5. customThe yellow precipitate formed
6. customis isolated by filtration
7. washrinsed with water
8. customdried in an oven
9. customAfter triturating in methanol
10. customdrying in an oven