Hydrazine, propyl- → HCID 54136901, Verbindung

HRID 1447797

Reaktionsgleichung

Reaktionsgleichung von HRID 1447797
[C:1]1([CH:7]=[C:8]2[C:13](=O)[C:12](=[CH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:11][S:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:22]([NH:25][NH2:26])[CH2:23][CH3:24]>CO>[C:1]1([CH:7]2[NH:26][N:25]([CH2:22][CH2:23][CH3:24])[C:13]3[C:12](=[CH:15][C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH2:11][S:10][CH2:9][C:8]2=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 42007Hydrazine, propyl-HCID 336779tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one

Produkt 1

HCID 54136901HCID 54136901, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of tetrahydro-3,5-bis-(phenylmethylene)-4H-thiopyran-4-one (5.84 g, 20 mmole) and n-propyl hydrazine (1.48 g, 20 mmole, CA 59:8724f) in MeOH (100 ml) is heated at reflux temperature for 3 hours. The initial heterogeneous mixture becomes homogeneous after about 0.5 hour. Upon cooling, crystals form and are collected and washed (MeOH) to give 5.0 g, m.p. 106°-118°. Recrystallization from MeOH gives the major product.

Aufarbeitung

  1. temperatureis heated
  2. temperatureat reflux temperature for 3 hours
  3. temperatureUpon cooling
  4. customcrystals form and are collected
  5. washwashed (MeOH)
  6. customto give 5.0 g, m.p. 106°-118°
  7. customRecrystallization from MeOH
  8. customgives the major product

Quellen und Nachweise

ORD-Eintrag
ord-c9dec93a8b574b648bb20e49d58eccb1
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04178379

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