Dimethylformamide → N-(2-acetoxy-3-phenoxypropyl) trichloroacetamidine hydrochloride
Reaktionsgleichung
C(N(CC)CC)C.Cl.[C:9]([O:12][CH:13]([CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:14][NH2:15])(=[O:11])[CH3:10].[Cl:24][C:25]([Cl:30])([Cl:29])[C:26](N)=[NH:27].CN(C)C=O>O>[ClH:24].[C:9]([O:12][CH:13]([CH2:16][O:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[CH2:14][NH:15][C:26](=[NH:27])[C:25]([Cl:30])([Cl:29])[Cl:24])(=[O:11])[CH3:10]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
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.
Aufarbeitung
- additionmixture of 1.23 g
- extractionextracted with benzene
- extractionThe benzene extract
- washis washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- dissolutionThe residue is dissolved in benzene
- additiontreated with an excess of ethanolic hydrogen chloride
- concentrationConcentration to dryness
Quellen und Nachweise
- ORD-Eintrag
- ord-04ec3107b7904c1f8865f7ad8b66703f
- Quelldatensatz
- uspto-grants-1977_12
- Patentnummer
- US04065465
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