Dimethylformamide → HCID 13051485, Verbindung

HRID 434767

Reaktionsgleichung

Reaktionsgleichung von HRID 434767
[S:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[NH:4][C:3](=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[C:12]([NH2:14])=[O:13])[CH2:2]1.[CH3:22]N(C=O)C.C(OC(OCC)N(C)C)C.COC(N(C)C)N(C)C>O>[F:21][C:18]1[CH:17]=[CH:16][C:15]([C:11]2[C:12](=[O:13])[NH:14][CH:22]=[C:2]3[C:3]=2[NH:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[S:1]3)=[CH:20][CH:19]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 709081-methoxy-N,N,N',N'-tetramethylmethylenediamineHCID 70913Dimethylformamide diethylacetalHCID 70532585HCID 70532585, Verbindung

Produkt 1

HCID 13051485HCID 13051485, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 4 parts of 2-(2H-1,4-benzothiazin-3(4H)-ylidene)-2-(4-fluorophenyl)acetamide in 80 parts of DMF is added 6 parts dimethylformamide diethyl acetal and the reaction mixture was stirred at room temperature for 2 to 6 hours then heated at 80°-140° C. for 1 to 6 hours. After cooling 6 parts of methoxy-bis-(dimethylamino)methane is added and the reaction mixture then heated at 50° to 80° C. for 2 to 24 hrs. The cooled reaction mixture is then diluted with 40 parts of water and refluxed for 2 to 18 hr. Upon cooling the precipitate present was collected and recrystallized from aqueous DMF to give 4-(4-fluorophenyl)-5H-pyrido[3,4-b][1,4]benzothiazin-3(2H)-one which melts above 300°.

Aufarbeitung

  1. temperaturethen heated at 80°-140° C. for 1 to 6 hours
  2. additionis added
  3. temperaturethe reaction mixture then heated at 50° to 80° C. for 2 to 24 hrs
  4. customThe cooled reaction mixture
  5. temperaturerefluxed for 2 to 18 hr
  6. temperatureUpon cooling the precipitate present
  7. customwas collected
  8. customrecrystallized from aqueous DMF

Quellen und Nachweise

ORD-Eintrag
ord-fb61a66ee3ca4ce6a6b4c4bd771f9a6a
Quelldatensatz
uspto-grants-1983_08
Patentnummer
US04399279

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