Ethyl Bromide → HCID 22722354, compound

Participants

Reaction Steps

15.00 g of 5,6-dihydroindeno[2,1-b]indole (99.8% by G.C., Mw=205.26, 73.1 mmol) were dissolved into 200 mL of 1,3-dioxolane (Aldrich) at room temperature in a 0.5-L flask. 8.28 g of t-BuOK (Fluka, 99%, Mw=112.22, 73.1 mmol) were added and the reaction mixture turned from a green suspension to a brown solution. After 30 min stirring at room temperature, 5.51 mL of EtBr (Fluka, 99%, Mw=108.97, d=1.46, 73.1 mmol) were added, obtaining a brown suspension. Stirring was continued for 2 hours, then the reaction mixture was poured into water containing 8 g of NH4Cl (Carlo Erba RPE, purity 99.5%). After two hours stirring, the green-brown suspension was filtered on a G4 frit, the solid dried in air under moderate vacuum to give a green powder (8.98 g), which was analyzed by 1H NMR. Purity 98.9% wt. by 1H NMR (yield=52.1%).

Provenance & Evidence