HCID 14516783, Verbindung → HCID 14516793, Verbindung

HRID 1762039Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1762039
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]([C:15]2[S:16][CH:17]=[N:18][N:19]=2)[C:10]=1[S:11]([NH2:14])(=[O:13])=[O:12])=[O:5])[CH3:2].[CH3:20][O:21][C:22]1[CH:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([N:30](C2C=CC=CC=2)[C:31](=O)[O-:32])[N:23]=1>C(#N)C>[CH3:29][O:28][C:26]1[CH:27]=[C:22]([O:21][CH3:20])[N:23]=[C:24]([NH:30][C:31]([NH:14][S:11]([C:10]2[N:9]([C:15]3[S:16][CH:17]=[N:18][N:19]=3)[CH:8]=[N:7][C:6]=2[C:4]([O:3][CH2:1][CH3:2])=[O:5])(=[O:13])=[O:12])=[O:32])[N:25]=1

Komponenten

4

Edukt 2

HCID 14516783HCID 14516783, VerbindungHCID 22104197HCID 22104197, Verbindung

Produkt 1

HCID 14516793HCID 14516793, VerbindungAusbeute 62,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

0.23 g of 1,8-diazobicyclo(5,4,0)-7-undecene was added dropwise to a mixture of 0.45 g of 4-ethoxycarbonyl-1-(1,3,4-thiadiazol-2-yl)imidazole-5-sulfonamide, 0.41 g of N-(4,6-dimethoxypyrimidine-2-yl)phenylcarbamate and 5 ml of acetonitrile. After stirring the reaction mixture at room temperature for 20 minutes, 20 ml of ice water was added thereto and the mixture was filtered. The filtrate was made acidic with use of conc. hydrochloric acid, and resulting precipitated crystals were collected by filtration, washed with water and ethyl ether, and dried to obtain 0.45 g of the title compound. m.p.: 169° to 171° C.

Aufarbeitung

  1. filtrationthe mixture was filtered
  2. customresulting
  3. customprecipitated crystals
  4. filtrationwere collected by filtration
  5. washwashed with water and ethyl ether
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9c8b4f252f3041eba5b5f04d0673f3a6
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04830660

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