反应详情

温度

0 °C

24.4 g (0.11 mol) of isopropyl (2Z)-3-hydroxy-2-cyano-4-ethyl-2-hexenoate were dissolved in CH2Cl2 and, at 25° C., 33.2 g (0.22 mol) of POCl3 were added. After cooling to 0° C., 43.8 g (0.44 mol) of triethylamine were added dropwise, and the mixture was stirred at 25° C. for 2 h. The solution was then concentrated and the residue was taken up in acetonitrile and cooled to 0° C., and 30 g (0.44 mol) of a 25 percent strength solution of ammonia were added dropwise. After 2 h of stirring, the mixture was concentrated to dryness, the residue was taken up in MTBE (methyl tert-butyl ether) and the organic phase was washed with NaOH and water, dried and concentrated. Purification by customary methods gave 10 g (40% of theory) of the title compound as a colorless solid (m.p. 140° C.).

1. concentrationThe solution was then concentrated
2. temperaturecooled to 0° C.
3. addition30 g (0.44 mol) of a 25 percent strength solution of ammonia were added dropwise
4. stirringAfter 2 h of stirring
5. concentrationthe mixture was concentrated to dryness
6. washthe organic phase was washed with NaOH and water
7. customdried
8. concentrationconcentrated
9. customPurification by customary methods