Sodium hydride → HCID 20434952, compound

Participants

Reaction Steps

Sodium hydride (0.19 g. of a 50% dispersion in oil) was added to a stirred solution of 2H-1,2,6-thiadiazine-1,1-dioxide (0.52 g) in dimethylformamide (4 cm3). After 0.5 hours 1-(6.7-dimethoxyquinazolin-4-yl)-4-(2-bromoethyl)piperidine (0.60 g) was added and the mixture was warmed at 70° for 10 hours. The solvent was removed in vacuo, water was added and the mixture was extracted with chloroform (4×20 cm3). The dried (MgSO4) extracts were evaporated and the residue was chromatographed on silica (Merck 60. 9385) eluting with methanol:ethyl acetate, 1:19, to give an oil which was crystallised from ethyl acetate to afford 1-(6,7-dimethoxyquinazolin-4-yl)-4-[2-(1,1-dioxo-1,2,6-thiadiazin-2-yl)ethyl]piperidine as microcrystals, m.p. 176°-8°, (0.18 g).

Provenance & Evidence