反应详情

A solution of anhydrous acetonitrile (2.3 g, 56 mmol) in THF (100 mL) was added dropwise at 80° C. to a mixture of NaH (60%, 2.8 g, 70 mmol) and methyl 2-cyano-2-methylpropanoate (6 g, 47 mmol) in THF (100 mL). The resultant reaction mixture was heated at reflux for 8 hours. The solvent was removed in vacuo and the residue was diluted with EtOAc and washed with 10% HCl, water and brine. The organics were dried (MgSO4) and concentrated in vacuo to obtain crude 2,2-dimethyl-3-oxopentanedinitrile (4 g), which was used for the next step reaction without further purification.

1. customThe resultant reaction mixture
2. temperaturewas heated
3. temperatureat reflux for 8 hours
4. customThe solvent was removed in vacuo
5. additionthe residue was diluted with EtOAc
6. washwashed with 10% HCl, water and brine
7. dry with materialThe organics were dried (MgSO4)
8. concentrationconcentrated in vacuo