Hydrazine hydrate (1:1) → N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide

HRID 1641440Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1641440
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:19])/[CH:13]=[CH:14]/[C:15](OC)=[O:16])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1>C(O)C>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([CH:13]2[CH2:14][C:15](=[O:16])[NH:3][NH:2]2)=[O:19])=[C:7]([C:20](=[O:27])[NH:21][CH:22]([CH:24]2[CH2:26][CH2:25]2)[CH3:23])[CH:6]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 44185603Methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxocrotonate

Produkt 1

HCID 44185604N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamideAusbeute 28,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A mixed liquid comprising 90 mg of hydrazine monohydrate and 3 ml of ethanol was added to a mixed liquid comprising 0.56 g of methyl 4-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylamino)-4-oxocrotonate and 3 ml of ethanol, followed by rinsing with 2 ml of ethanol, and reflux under heating for 6 hours. The reaction liquid was stood to cool, the precipitated crystals were subjected to suction filtration, and the obtained crystals were washed with ethanol and air dried to obtain 0.16 g of the desired product (melting point: 248° C.).

Aufarbeitung

  1. additionwas added to a mixed liquid
  2. washby rinsing with 2 ml of ethanol
  3. temperaturereflux
  4. temperatureunder heating for 6 hours
  5. customThe reaction liquid
  6. temperatureto cool
  7. filtrationthe precipitated crystals were subjected to suction filtration
  8. washthe obtained crystals were washed with ethanol and air
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-8129bd76f647472bbf94c736d024e31b
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08115006B2

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