Dimethylformamide → HCID 66767080, Verbindung

HRID 1661990Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1661990
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:7]([CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][O:17]1)[N:6]=[CH:5]2.F[C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][C:24]=1[F:32].C([O-])(O)=O.[Na+].CN(C=O)C>O>[CH2:14]([O:13][C:11]([C:10]1[CH:9]=[C:8]2[C:4]([CH:5]=[N:6][N:7]2[CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)=[CH:3][C:2]=1[O:1][C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][C:24]=1[F:32])=[O:12])[CH3:15]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 516892Sodium BicarbonateHCID 66766901HCID 66766901, Verbindung

Produkt 1

HCID 66767080HCID 66767080, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of ethyl 5-hydroxy-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-6-carboxylate (10.8 g, 37 mmol), 1,2-difluoro-4-nitrobenzene (7.1 g, 44 mmol), NaHCO3 (7.4 g, 88 mmol) and DMF (100 mL) is stirred at 80° C. for 2 hours. After it is cooled to RT, water (400 mL) and PE (50 mL) are added and the mixture is stirred for 20 min. The precipitate is collected and dried under vacuum at 50° C. to afford the product (15 g, 95% yield). MS (m/z): 430.1 (M+H).

Aufarbeitung

  1. temperatureAfter it is cooled to RT
  2. stirringthe mixture is stirred for 20 min
  3. customThe precipitate is collected
  4. customdried under vacuum at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-e185d7f75c9f43de8213fe4791143681
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08030302B2

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