Tributylvinyltin → HCID 18670535, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 0.30 g of 8-(6-chloropurin-7-ylmethyl)-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine in N,N-dimethylformamide (10 ml) were added in a nitrogen atmosphere 0.312 g of vinyl-tri-n-butyltin (IV) and 0.050 g of bis(triphenylphosphine) palladium (II) chloride. After degassing, the mixture was heated to 80° C. for 20 hours. Then the insoluble matters were removed by filtering through celite. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 0.19 g of 10-methoxymethyl-8-(6-vinylpurin-7-ylmethyl)-10H-pyrazino[2,3-b][1,4]benzothiazine as a yellow solid. To a solution of 190 mg of the obtained compound in methanol (20 ml) was added 0.018 g of palladium/carbon and hydrogenation was effected in a hydrogengas stream for 2 hours. Thus, 0.10 g of the title compound was obtained as a yellow solid.

Provenance & Evidence