反应详情

To a solution of 8.0 g (0.027 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione in 50 ml of absolute ethanol was added 6 ml (0.054 mole) of 40% aqueous solution of dimethylamine. The solution was heated in a steel bomb at 90° C. for 14 hr. The ethanol was removed under reduced pressure and the residue was partitioned between chloroform and aqueous sodium hydroxide. The chloroform layer was concentrated to give a viscous yellow oil. The oil was dissolved in isopropyl alcohol and reacted with oxalic acid. The oxalate salt immediately precipitated. The mixture was heated and a small amount of water was added to dissolve the salt. A white crystalline powder was obtained, m.p. 150°-151° C.

1. customThe ethanol was removed under reduced pressure
2. customthe residue was partitioned between chloroform and aqueous sodium hydroxide
3. concentrationThe chloroform layer was concentrated
4. customto give a viscous yellow oil
5. customThe oxalate salt immediately precipitated
6. temperatureThe mixture was heated
7. additiona small amount of water was added
8. dissolutionto dissolve the salt
9. customA white crystalline powder was obtained