反应详情

41.5 G. of 1-carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine are reacted together with 1 l. of absolute diglyme (diethyleneglycoldimethylether) with 26.5 g. of sodium borohydride and stirred at 25° for 30 minutes. The reaction mixture is then mixed dropwise at 20°-30° over a 45-minute period with a solution of 138.6 g. of oxalic acid in 800 ml. of diglyme. The reaction mixture is maintained at 100° for 15 hours. The resulting mixture is evaporated under reduced pressure. The residue is suspended in 1 l. of 2N aqueous sodium hydroxide and extracted with benzene. The benzene extract is washed with water, dried and evaporated, whereby there is obtained 1-carbethoxy-4-(8-chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine as a red-brown oil, whose nmr and ir spectra are consistent with the proposed structure.

1. additionThe reaction mixture is then mixed dropwise at 20°-30° over a 45-minute period with a solution of 138.6 g
2. temperatureThe reaction mixture is maintained at 100° for 15 hours
3. customThe resulting mixture is evaporated under reduced pressure
4. extractionof 2N aqueous sodium hydroxide and extracted with benzene
5. extractionThe benzene extract
6. washis washed with water
7. customdried
8. customevaporated