Methane → HCID 20529046, Verbindung

HRID 66766

Reaktionsgleichung

Reaktionsgleichung von HRID 66766
[C:1]([C:3]1[CH:12]=[CH:11][C:6]([O:7][CH2:8][C:9]#[N:10])=[CH:5][CH:4]=1)#[N:2].[C:13]1([CH3:23])[CH:18]=[CH:17][C:16]([S:19]([OH:22])(=[O:21])=[O:20])=[CH:15][CH:14]=1.[CH2:24](N)[CH2:25][NH2:26].C(O)C.C>ClC1C=CC=CC=1Cl.C(Cl)Cl.O>[C:13]1([CH3:23])[CH:14]=[CH:15][C:16]([S:19]([OH:22])(=[O:20])=[O:21])=[CH:17][CH:18]=1.[C:1]([C:3]1[CH:12]=[CH:11][C:6]([O:7][CH2:8][C:9]2[NH:26][CH2:25][CH2:24][N:10]=2)=[CH:5][CH:4]=1)#[N:2]

Komponenten

8

Edukt 4

HCID 297Methane2×HCID 702EthanolHCID 2250301,2-Ethanediamine, 4-methylbenzenesulfonate (1:?)HCID 205290614-(Cyanomethoxy)benzonitrile

Produkt 1

HCID 20529046HCID 20529046, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 72391,2-DichlorobenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

A mixture of 15.8 g of 4-cyanophenoxyacetonitrile and 23.3 g of ethylenediamine p-toluenesulfonate in 50 ml of 1,2-dichlorobenzene was heated at from about 130°-145° C. for about an hour. After reaction the mixture was cooled, diluted with CH2Cl2 and filtered to obtain the crude product. The crude product was dissolved in boiling absolute ethanol, treated with activated charcoal and filtered through a fluted paper. The filtrate was cooled to 5° C. for 1.5 hours and the crystals which formed removed by filtering. After drying in a vacuum oven, off-white crystals were obtained having a melting point of 190°-192° C. The off-white crystals were put in solution in 200 ml of boiling water and treated with activated charcoal and filtered. The filtrate was cooled to 5° C. for 1 hour and the crystals which formed removed by filtration. Upon drying, the product 2-((4-cyanophenoxy)methyl)-2-imidazoline p-toluenesulfonate was obtained as white crystals, m.p. 196°-198° C.

Aufarbeitung

  1. temperaturewas heated at from about 130°-145° C. for about an hour
  2. customAfter reaction the mixture
  3. temperaturewas cooled
  4. filtrationfiltered
  5. customto obtain the crude product
  6. filtrationfiltered through a fluted paper
  7. customthe crystals which formed
  8. customremoved
  9. filtrationby filtering
  10. customAfter drying in a vacuum oven
  11. customoff-white crystals were obtained
  12. filtrationfiltered
  13. temperatureThe filtrate was cooled to 5° C. for 1 hour
  14. customthe crystals which formed
  15. customremoved by filtration
  16. customUpon drying

Quellen und Nachweise

ORD-Eintrag
ord-eb7a0cf14e554f1c8b942e4242ebdfe8
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04343808

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