Sodium hydride → HCID 20266386, compound

Participants

Reaction Steps

Sodium hydride (2.5 g of a 50% dispersion in oil) was added to a stirred suspension of 1-[4-toluenesulphonyloxy]-2-[1-(6,7-dimethoxyquinazolin-4-yl)piperid-4-yl]-2-hydroxypropane (8.6 g) in THF (20 cm3) and the mixture was heated under reflux for 16 hours. Volatile material was removed in vacuo, the residue was partitioned between chloroform (50 cm3) and water (50 cm3) and the aqueous phase was further extracted with chloroform (2×50 cm3). The combined, dried (MgSO4) organic phase was evaporated and the residue was crystallized from ethyl acetate to afford 2-methyl-2-[1-(6,7-dimethoxy-quinazolin-4-yl)piperid-4-yl]oxirane, m.p. 125°-127.5° (5.0 g).

Provenance & Evidence