5-chloro-5,6-dihydrobenzo[b][1]benzothiepine

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10-Chloro-10,11-dihydrodibenzo[b,f]thiepine (10 g, 0.041 mol, prepared as described in Monatshefte 96, 182, 1965) was slowly added to a mixture of 2-bromoethanol (44 g, 0.35 mol) and powdered potassium carbonate (10 g, 0.072 mol) at room temperature. After stirring for 6 h, dichloromethane (15 ml) was added, and the reaction mixture was heated at 50° C. for 3 h. After cooling, dichloromethane (35 ml) was added and the mixture was filtered. The dichloromethane was evaporated and excess of 2-bromoethanol was distilled off in vacuo. The oily residue was dissolved in benzene (100 ml), washed with water (3×70 ml), dried (K2CO3) and the solvent was evaporated to give 13.8 g of crude 10-(2-bromoethoxy)-10,11-dihydrodibenzo[b,f]thiepine as an oil. After cooling the mixture was filtered The dichloromethane was evaporated and excess of 2-bromoethanol was distilled off in vacuo The oily residue was dissolved in benzene (100 ml) washed with water (3×70 ml) dried (K2CO3) the solvent was evaporated

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10-Chloro-10,11-dihydrodibenzo[b,f]thiepine (10 g, 0.041 mol, prepared as described in Monatshefte 96, 182, 1965) was slowly added to a mixture of 2-bromoethanol (44 g, 0.35 mol) and powdered potassium carbonate (10 g, 0.072 mol) at room temperature. After stirring for 6 h, dichloromethane (15 ml) was added, and the reaction mixture was heated at 50° C. for 3 h. After cooling, dichloromethane (35 ml) was added and the mixture was filtered. The dichloromethane was evaporated and excess of 2-bromoethanol was distilled off in vacuo. The oily residue was dissolved in benzene (100 ml), washed with water (3×70 ml), dried (K2CO3) and the solvent was evaporated to give 13.8 g of crude 10-(2-bromoethoxy)-10,11-dihydrodibenzo[b,f]thiepine as an oil. After cooling the mixture was filtered The dichloromethane was evaporated and excess of 2-bromoethanol was distilled off in vacuo The oily residue was dissolved in benzene (100 ml) washed with water (3×70 ml) dried (K2CO3) the solvent was evaporated