Hydrochloric Acid → 1,2-Dihydro-N-(2,4-difluorophenyl)-1-oxopyrrolo[3,2,1-kl]phenothiazine-2-carboxamide

HRID 1653664Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1653664
[H-].[Na+].[C:3]1(=[O:19])[N:17]2[C:18]3[C:9]([S:10][C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=42)=[CH:8][CH:7]=[CH:6][C:5]=3[CH2:4]1.[F:20][C:21]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=1[N:28]=[C:29]=[O:30].Cl>CN(C=O)C>[F:20][C:21]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=1[NH:28][C:29]([CH:4]1[C:5]2[CH:6]=[CH:7][CH:8]=[C:9]3[S:10][C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=4[N:17]([C:18]=23)[C:3]1=[O:19])=[O:30]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 5932582,4-Difluorophenyl isocyanateHCID 14459974HCID 14459974, Verbindung

Produkt 1

HCID 144599751,2-Dihydro-N-(2,4-difluorophenyl)-1-oxopyrrolo[3,2,1-kl]phenothiazine-2-carboxamideAusbeute 360,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a suspension of sodium hydride (0.14 g) in DMF (10 ml) was added pyrrolo[3,2,-1kl]phenothiazine-1-one (0.48 g) and to the resulting solution was slowly added 2,4-difluorophenyl isocyanate (0.31 g) . The reaction mixture was stirred for 12 hours and then poured onto ice water (50 ml). The resulting mixture was acidified to pH 2.0 with 6N HCl and the precipitated solid was collected and then air dried-to yield the title compound (2.84 g). A sample recrystallized from methylene chloride had a m.p. of 208°-209° C.

Aufarbeitung

  1. additionpoured onto ice water (50 ml)
  2. customthe precipitated solid was collected
  3. customair dried-to

Quellen und Nachweise

ORD-Eintrag
ord-3ad204e6951346df9886b336521d5a41
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05403839

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