Hydrazine hydrate (1:1) → 4-(4-chloro-3-methylphenyl)-1H-pyrazole-3,5-diamine

HRID 1912899Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1912899
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]([C:14]#[N:15])[C:12]#[N:13])=[CH:7][C:6]=1[CH3:16]>C(Cl)(Cl)Cl>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:14]([NH2:15])=[N:2][NH:3][C:12]=2[NH2:13])=[CH:7][C:6]=1[CH3:16]

Komponenten

4

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Hydrazine monohydrate (0.312 mL, 6.4 mmol) was added to a solution of the product from Example 47A (512 mg, 2.69 mmol) in CHCl3 (25 mL). The reaction flask was evacuated and purged with nitrogen (3 cycles) and the mixture was heated at 70° C. under nitrogen for 22 hours, then cooled to room temperature. The mixture was concentrated under vacuum to provide the title compound as a beige solid. MS (DCI/NH3) m/z 223/225 (M+H)+.

Aufarbeitung

  1. customThe reaction flask was evacuated
  2. custompurged with nitrogen (3 cycles)
  3. temperaturecooled to room temperature
  4. concentrationThe mixture was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a4e073b01ed3423fab9e38b75e8a600e
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08609669B2

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