Hydrazine, propyl- → 2,4,6,7-Tetrahydro-3-(4-methylphenyl)-7-[(4-methylphenyl)-methylene]-1-propylthiopyrano[4,3-c]pyrazole

HRID 1447803Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1447803
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[C:9]2[C:14](=O)[C:13](=[CH:16][C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=3)[CH2:12][S:11][CH2:10]2)=[CH:4][CH:3]=1.[CH2:24]([NH:27][NH2:28])[CH2:25][CH3:26]>CO>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[NH:28][N:27]([CH2:24][CH2:25][CH3:26])[C:14]3[C:13](=[CH:16][C:17]4[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=4)[CH2:12][S:11][CH2:10][C:9]2=3)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 42007Hydrazine, propyl-HCID 545668043,5-Bis[(4-methylphenyl)methylidene]thian-4-one

Produkt 1

HCID 545277492,4,6,7-Tetrahydro-3-(4-methylphenyl)-7-[(4-methylphenyl)-methylene]-1-propylthiopyrano[4,3-c]pyrazoleAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of tetrahydro-3,5-bis-(4-methylphenylmethylene)-4H-thiopyran-4-one (6.7 g, 20 mmole) and n-propylhydrazine (1.6 g, 22 mmole) in methanol (250 ml) is heated at reflux temperature for 5 hours, then cooled overnight. The pale yellow precipitate is collected by filtration. The filtrate is concentrated to about 50 ml and additional precipitate is again collected by filtration and combined with the previous batch to give 5.5 g of a crude product mixture.

Aufarbeitung

  1. temperatureis heated
  2. temperatureat reflux temperature for 5 hours
  3. temperaturecooled overnight
  4. filtrationThe pale yellow precipitate is collected by filtration
  5. concentrationThe filtrate is concentrated to about 50 ml and additional precipitate
  6. filtrationis again collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-014daa33d227416dab316ccf793bb426
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04178379

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