Reaktion #549238

Reaktionsgleichung

dimethylformamide

Triethylamine

2-acetoxy-3-phenoxy-propylamine hydrochloride

trichloroacetamidine

→

N-(2-acetoxy-3-phenoxypropyl) trichloroacetamidine hydrochloride

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONmixture of 1.23 g
2. 2
   Extraktionextracted with benzene
3. 3
   ExtraktionThe benzene extract
4. 4
   Waschenis washed with water
5. 5
   Trocknendried over magnesium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated
8. 8
   workup.DISSOLUTIONThe residue is dissolved in benzene
9. 9
   workup.ADDITIONtreated with an excess of ethanolic hydrogen chloride
10. 10
    EinengenConcentration to dryness

Vorschrift

Triethylamine (0.50 g., 5.0 mmoles) is added in small portions over 10 minutes to a well stirred mixture of 1.23 g. (5.0 mmoles) of 2-acetoxy-3-phenoxy-propylamine hydrochloride and 1.61 g. (10 mmoles) of trichloroacetamidine in 5 ml. of dimethylformamide. The reaction mixture is heated at 60° C. for 2 hours, diluted with water and extracted with benzene. The benzene extract is washed with water, dried over magnesium sulfate, filtered and concentrated. The residue is dissolved in benzene and treated with an excess of ethanolic hydrogen chloride. Concentration to dryness affords N-(2-acetoxy-3-phenoxypropyl) trichloroacetamidine hydrochloride with a m.p. of 70° to 77° C.

Quelle