Water → N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate

HRID 1288226

Reaktionsgleichung

Reaktionsgleichung von HRID 1288226
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([OH:10])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[O:12]([CH:19]([CH3:22])[CH2:20][NH2:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C:23]1([CH2:29][C:30]#[N:31])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O.CCOCC>C(O)C>[C:1]1([CH3:11])[CH:2]=[CH:3][C:4]([S:7]([OH:10])(=[O:8])=[O:9])=[CH:5][CH:6]=1.[O:12]([CH:19]([CH3:22])[CH2:20][NH:21][C:30](=[NH:31])[CH2:29][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 3283Diethyl EtherHCID 8794PhenylacetonitrileHCID 215043372-Phenoxypropylamine p-toluenesulphonate

Produkt 1

HCID 178457535N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2-phenoxypropylamine p-toluenesulphonate (3.7 g.) and phenylacetonitrile (1.5 g.) was stirred and heated, in an oil-bath, to 270° for 11/2 hours. The mixture was cooled and dissolved in the minimum amount of boiling ethanol, and the solution was poured into a mixture of water (75 ml.) and ether (75 ml.). The mixture was shaken and the aqueous layer was separated, washed once with ether, and evaporated to half-volume under reduced pressure. An oil separated and crystallised after a few days. The product was filtered and recrystallised from water to give N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate, m.p. 121°-124°.

Aufarbeitung

  1. temperatureheated, in an oil-bath, to 270° for 11/2 hours
  2. temperatureThe mixture was cooled
  3. stirringThe mixture was shaken
  4. customthe aqueous layer was separated
  5. washwashed once with ether
  6. customevaporated to half-volume under reduced pressure
  7. customAn oil separated
  8. customcrystallised after a few days
  9. filtrationThe product was filtered
  10. customrecrystallised from water

Quellen und Nachweise

ORD-Eintrag
ord-25956d0a3e5442a3b3867d8419a2d4b4
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03987158

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