Hydrochloric Acid → HCID 178493668, Verbindung

HRID 37135

Reaktionsgleichung

Reaktionsgleichung von HRID 37135
[H-].[Na+].[CH:3]([O:5][CH2:6][CH3:7])=O.[CH3:8][O:9]CC(OCC)=O.[NH2:16][C:17]1[C:21]([C:22]2[CH:27]=[CH:26][C:25]([S:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:24][CH:23]=2)=[CH:20][NH:19][N:18]=1.Cl>C(OCC)(=O)C.O.O1CCCC1>[OH:9][C:8]1[N:18]2[N:19]=[CH:20][C:21]([C:22]3[CH:23]=[CH:24][C:25]([S:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:26][CH:27]=3)=[C:17]2[N:16]=[CH:7][C:6]=1[O:5][CH3:3]

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 77544Ethyl 2-methoxyacetateHCID 178509258HCID 178509258, Verbindung

Produkt 1

HCID 178493668HCID 178493668, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.0 g of ethyl methoxyacetate were added under nitrogen atmosphere, and the mixture was stirred for 16 hours at room temperature. In succession, adding 1.0 g of 3-amino-4(4-phenylthiophenyl)pyrazole, the solution was stirred for 4 hours in reflux. After allowing to cool, water was added and the solution was neutralized with 10% hydrochloric acid. Removing water, ethyl acetate was added, and insoluble matter was filtered. The filtrate was washed in ethyl acetate and ether and dried, and the title compound was obtained (100 mg, 8%).

Aufarbeitung

  1. additionwere added under nitrogen atmosphere
  2. stirringthe solution was stirred for 4 hours
  3. temperaturein reflux
  4. temperatureto cool
  5. filtrationinsoluble matter was filtered
  6. washThe filtrate was washed in ethyl acetate
  7. dry with materialether and dried

Quellen und Nachweise

ORD-Eintrag
ord-907f2ec5246641ac9182ba93481bc4bb
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420128

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