Acetic Acid → HCID 178527782, Verbindung

HRID 1199337

Reaktionsgleichung

Reaktionsgleichung von HRID 1199337
CO[C:3]1[C:9](=O)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[NH2:11][C:12]([NH2:14])=[S:13].C[O-].[Na+].C(O)(=O)C>CO>[SH:13][C:12]1[N:11]=[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=[C:9]2[N:14]=1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 165462-Methoxy-2,4,6-cycloheptatrien-1-oneHCID 2723790ThioureaHCID 10942334Sodium Methoxide

Produkt 1

HCID 178527782HCID 178527782, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

According to the method disclosed in Journal of the American Chemical Society, vol. 76, pages 3352 and 3353 (1954), 150 g of 2-methoxytropone and 84 g of thiourea were added to 255 g of a solution of 28% sodium methoxide in methanol, and stirred at room temperature for 30 minutes. Further, 600 ml of methanol was added thereto and acetic acid was added until the pH of the solution becomes around 5. Deposited crystals were filtered and washed with methanol. The obtained crystals were added to 1 l of methanol, and refluxed with heating for 30 minutes. After being allowed to cool to room temperature, the crystals were filtered and dried.

Aufarbeitung

  1. filtrationDeposited crystals were filtered
  2. washwashed with methanol
  3. additionThe obtained crystals were added to 1 l of methanol
  4. temperaturerefluxed
  5. temperaturewith heating for 30 minutes
  6. temperatureto cool to room temperature
  7. filtrationthe crystals were filtered
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ea45f1326eab45b0a956340c01cdb20a
Quelldatensatz
uspto-grants-1990_02
Patentnummer
US04900648

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