Reacción #1551007

Ecuación de reacción

Dimethylsulphate

8-morpholinooctylamine

sodium hydroxide

→

N-(morpholinyloctyl),N-methylamine

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONthe temperature being kept below 70° C. throughout the addition
2. 2
   workup.STIRRINGStirring
3. 3
   Temperaturaheated to boiling
4. 4
   workup.WAITAfter two hours
5. 5
   OtroAn oil was separated which
6. 6
   Otrothe mixture obtained
7. 7
   Otrowas dried on Na2SO4
8. 8
   Otroevaporated under reduced pressure
9. 9
   OtroThe collected residue was purified by silica gel chromatography
10. 10
    Lavadoeluting with CHCl3 /MeOH/NH4OH, 65:35:2
11. 11
    Otroto separate the desired product of very intense colour by ninhydrin and iodine reactions

Procedimiento

Dimethylsulphate (832 mg; 0.66 mmoles) was slowly added to 8-morpholinooctylamine (141 mg; 0.66 mmoles) under stirring, the temperature being kept below 70° C. throughout the addition. Stirring was continued overnight. Then the mixture was treated with sodium hydroxide solution (880 mg) in water (15 ml) and heated to boiling. After two hours, the mixture was cooled to room temperature. An oil was separated which was combined with the water layer benzene extracts: the mixture obtained was dried on Na2SO4 and evaporated under reduced pressure. The collected residue was purified by silica gel chromatography, eluting with CHCl3 /MeOH/NH4OH, 65:35:2, to separate the desired product of very intense colour by ninhydrin and iodine reactions.

Fuente