Dimethylformamide → HCID 66767080, Verbindung

HRID 2195506Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2195506
[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-e9bad44593d246de84a4977cf428ddd7
Quelldatensatz
uspto-grants-2012_12
Patentnummer
USRE043878E1

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