Tributylstannane → HCID 12621140, compound

Participants

Reaction Steps

A mixture of 8.07 g of 1a, 17.2 g of freshly distilled tributyltin hydride and 50 ml of anhydrous benzene is heated under reflux under nitrogen for 3 days. Most of the benzene is removed and the residue is distilled through a short-path column (to 125° bath temperature, 1 micron). The pot residue is crystallized from isopropyl alcohol to give 3,63 g (71% yield) of 2-methyl-2,3,8,12b-tetrahydro-1H-3a,8-methanodibenzo[3,4:6,7]cyclohepta[1,2-c]pyrrol-1-one (1b), mp 141°-146°. A sample crystallized once from isopropyl alcohol has mp 147°-157°.

Provenance & Evidence