Sodium hydride → HCID 67884120, compound

Participants

Reaction Conditions

Reaction Steps

7.85 g (56 mmol) of 2-hydroxy-5-nitro-pyridine are added in portions to 1.61 g (56 mmol) of sodium hydride (80% dispersion in mineral oil) in 30 ml of DMPU (1,3-dimethyl-tetrahydro-2(1H)-pyrimidinone) under argon. After evolution of gas has ceased the mixture is stirred for 20 minutes. Then, at room temperature, a solution of 4,5-epoxy-2,3,4,5-tetrahydro-1-benzoxepin in 10 ml of DMPU is added dropwise. The mixture is subsequently heated at 95° C. for 6 hours. The mixture is poured into ice/water, stirring vigorously, and precipitated solid is filtered off with suction. The solid is chromatographed on silica gel (ethyl acetate/cyclohexane 2:1), and the pale yellow oil obtained in this way is crystallized in methyl tert.-butyl ether. Melting point 152°-155° C.

Provenance & Evidence