Water → HCID 21435163, compound

Participants

Reaction Steps

24.5 g of 4-(1-methyl-4-piperidylidene)-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-10(9H)-one were dissolved in 750 ml of boiling cyclohexane. The mixture was cooled to 50° and whilst this temperature was maintained 10.7 g of potassium tert-butylate were added. The resulting suspension was cooled to 20°, and whilst this temperature was maintained 12.4 g of methyl iodide were slowly added dropwise. The mixture was stirred for a further 1 hour and then treated with 100 ml of water and 100 ml of benzene. The organic phase was separated off and evaporated to yield crude 9-methyl-4-(1-methyl-4-piperidylidene)-4H-benzo[4,5]cyclohepta[1,2-b]thiophene-10(9H)-one as an oil which can be used further in crude form (M.Pt. of hydrogen fumarate 213°-215° from ethanol).

Provenance & Evidence