تفاعل #334491

معادلة التفاعل

7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

dimethylamine

oxalic acid

→

7-Chloro-2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione oxalate hydrate

المذيبات

isopropyl alcohol

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe ethanol was removed under reduced pressure
2. 2
   أخرىthe residue was partitioned between chloroform and aqueous sodium hydroxide
3. 3
   تركيزThe chloroform layer was concentrated
4. 4
   أخرىto give a viscous yellow oil
5. 5
   أخرىThe oxalate salt immediately precipitated
6. 6
   درجة الحرارةThe mixture was heated
7. 7
   workup.ADDITIONa small amount of water was added
8. 8
   workup.DISSOLUTIONto dissolve the salt
9. 9
   أخرىA white crystalline powder was obtained

الإجراء التجريبي

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, mp. 150°-151° C.

المصدر