反应详情

温度

120 °C

To a solution of 2.0 g of 10,11-dihydro-10-(4-iodobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine and 4.39 g of 2-[(tri-n-butyl)stannyl]pyridine in 30 ml of toluene under nitrogen is added 0.2 g of tetrakis(triphenylphosphine)palladium and the mixture heated to 120° C. for 16 hours. The toluene is evaporated in vacuo and the oily residue diluted with 50 ml of chloroform and washed with water, dried (Na2SO4), filtered through diatomaceous earth and evaporated in vacuo to give a residue which is columned on silica gel by elution with 7:1 to 1:1 ethyl acetate:hexane to give 1.44 g of the desired product as a solid, m.p. 170°-172° C.; M+H=366.1; M+Na=388.1.

1. customThe toluene is evaporated in vacuo
2. additionthe oily residue diluted with 50 ml of chloroform
3. washwashed with water
4. dry with materialdried (Na2SO4)
5. filtrationfiltered through diatomaceous earth
6. customevaporated in vacuo
7. customto give a residue which
8. washis columned on silica gel by elution with 7:1 to 1:1 ethyl acetate