Methane → HCID 178428206, Verbindung

HRID 268244

Reaktionsgleichung

Reaktionsgleichung von HRID 268244
Cl.N([C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1)C1C=CC=CC=1.[Cl:23][C:24]1[CH:25]=[C:26]([CH:28]=[CH:29][C:30]=1[CH3:31])[NH2:27].C(O)C.C>CO>[ClH:23].[Cl:23][C:24]1[CH:25]=[C:26]([CH:28]=[CH:29][C:30]=1[CH3:31])[NH:27][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1

Komponenten

6

Edukt 4

HCID 297MethaneHCID 702EthanolHCID 72553-Chloro-4-methylanilineHCID 178428198HCID 178428198, Verbindung

Produkt 1

HCID 178428206HCID 178428206, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A 500 ml., 3-neck, r.b. flask fitted with stirrer, condenser, and thermometer was charged with a mixture of the compound of Example I, C. (21.7 g., 0.1 mole), 3-chloro-4-methylaniline (14.2 g., 0.1 mole) and ethanol (300 ml.). The mixture was heated at reflux, while stirring, overnight. The near solution was concentrated to dryness by rotary evaporator and the residue was collected and dried to yield 35 g. (97.5%), m.p. 352°-364°C (dec). A 10 g. sample was dissolved in methanol (200 ml.), treated with charcoal and filtered while hot. Ether (ca 750 ml.) was added until the filtrate remained turbid and was then chilled. The crystals were collected by filtration and dried to yield 3.4 g. yellow crystals, m.p. 362°-370°C (dec). After two recrystallizations a m.p. 368°-372°C (dec) was obtained.

Aufarbeitung

  1. customflask fitted with stirrer, condenser
  2. temperatureThe mixture was heated
  3. temperatureat reflux
  4. concentrationThe near solution was concentrated to dryness by rotary evaporator
  5. customthe residue was collected
  6. customdried
  7. customto yield 35 g
  8. filtrationfiltered while hot
  9. additionEther (ca 750 ml.) was added until the filtrate
  10. temperaturewas then chilled
  11. filtrationThe crystals were collected by filtration
  12. customdried
  13. customto yield 3.4 g
  14. customAfter two recrystallizations a m.p. 368°-372°C (dec)
  15. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-b80aeb6711fb4a458f42da2f0091e636
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03947434

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