Réaction #54280

Équation de réaction

1-(3,4-methylenedioxyphenyl)-2-chloroethanol

ethylamine

→

1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

Solvants

ethanol

Conditions de réaction

Traitement

1. 1
   TempératureAfter cooling
2. 2
   workup.DISTILLATIONthe ethanol and excess ethylamine are distilled off under reduced pressure
3. 3
   ExtractionThe residue is extracted with 100 ml
4. 4
   Lavageof 1N HCl and the extract is washed twice with 100 ml
5. 5
   ExtractionThe hydrochloric acid extract solution
6. 6
   Extractionthe liberated oil is extracted with ether
7. 7
   ExtractionThe ether extract
8. 8
   Autreis dried
9. 9
   workup.ADDITIONan etherial hydrochloric acid solution is added
10. 10
    Filtrationare filtered off
11. 11
    Lavagewashed with ether
12. 12
    AutreUpon recrystallization from isopropyl alcohol 7.8 g

Mode opératoire

19.5 g. of 1-(3,4-methylenedioxyphenyl)-2-chloroethanol are added to a solution of 170 g. of ethylamine in 200 ml. of cooled ethanol and the mixture is heated at 80° C. for 8 hours in an autoclave. After cooling, the ethanol and excess ethylamine are distilled off under reduced pressure. The residue is extracted with 100 ml. of 1N HCl and the extract is washed twice with 100 ml. of ether. The hydrochloric acid extract solution is made basic with 1N caustic soda and the liberated oil is extracted with ether. The ether extract is dried and an etherial hydrochloric acid solution is added thereto. The crystals which settle out on standing are filtered off and washed with ether. Upon recrystallization from isopropyl alcohol 7.8 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained.

Source