反应详情

2-(2-Cyanoethyl)malonic acid diethyl ester (148.3 g) was reacted with sodium hydride (15.3 g) in tetrahydrofuran at 20° C. 2-Chloro-3-methyl-5-nitropyridine (100 g) was added and the internal temperature was raised to 100° C. (some tetrahydrofuran was distilled off) over 14 hrs. The reaction mixture was partitioned between water and chloroform, the chloroform extract was dried, treated with charcoal and filtered through a silica bed and then evaporated to dryness. Crystallisation of the residue from ethanol gave 4-(3-methyl-5-nitropyrid-2-yl)-4,4-bis(carbethoxy)-butyronitrile (99 g) m.p. 64°-65.5° C.

1. distillationwas distilled off) over 14 hrs
2. customThe reaction mixture was partitioned between water and chloroform
3. extractionthe chloroform extract
4. customwas dried
5. additiontreated with charcoal
6. filtrationfiltered through a silica bed
7. customevaporated to dryness
8. customCrystallisation of the residue from ethanol