反应详情

A solution of KCN (3g, 0.046 mol) in a minimum of water was added to a solution of benzo[b]quinolizinium bromide (10 g; 0.0385 mol) in 200 ml water. The resulting solid was extracted with an equal volume of methylene chloride. The above organic layer was heated and a solution of bromine (6.4 g) in methylene chloride was added. The resulting yellow solid was isolated, dissolved in ethanol/water, and the resulting solution was treated with sodium perchlorate solution. The perchlorate salt was filtered and recrystallized from ethanol to afford 2 g of 6-cyano-benzo[b]quinolizinium perchlorate (Formula II: R1 =R7 =H; R2 =CN; X- =ClO4-) as a solid.

1. extractionThe resulting solid was extracted with an equal volume of methylene chloride
2. temperatureThe above organic layer was heated
3. additiona solution of bromine (6.4 g) in methylene chloride was added
4. customThe resulting yellow solid was isolated
5. filtrationThe perchlorate salt was filtered
6. customrecrystallized from ethanol