反应详情

温度

95 °C

A solution of the crude product from step A dissolved in 80 mL of DMF containing 4.4 mL methanol and 4.61 g cyanoacetamide was transferred by cannula into a flask containing a suspension of NaH (4.98 g, 60% dispersion in mineral oil, freed of excess oil by washing with hexane just prior to use) in DMF (40 mL). The solution was heated to 95° C. for 2.5 hours then concentrated. The residue was dissolved in ethyl acetate, washed twice with 10% aqueous NaHSO4, and twice with water before concentrating to a solid. The solid was suspended in warm ethanol and then cooled, and the title compound was subsequently isolated by filtration and dried in vacuo.

1. additioncontaining
2. washby washing with hexane just
3. concentrationthen concentrated
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed twice with 10% aqueous NaHSO4
6. concentrationtwice with water before concentrating to a solid
7. temperaturecooled