Sodium Carbonate → HCID 57551211, Verbindung

HRID 1644649Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1644649
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:12][NH2:13])=O)=[CH:5][CH:4]=1.[N:16]([C:19]1[CH:24]=[CH:23][C:22]([S:25]([NH:28][C:29]2[S:30][CH:31]=[CH:32][N:33]=2)(=[O:27])=[O:26])=[CH:21][CH:20]=1)=[C:17]=[S:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[S:30]1[CH:31]=[CH:32][N:33]=[C:29]1[NH:28][S:25]([C:22]1[CH:21]=[CH:20][C:19]([NH:16][C:17]2[S:18][C:10]([CH2:9][C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:15])([F:14])[F:1])=[CH:4][CH:5]=3)=[N:12][N:13]=2)=[CH:24][CH:23]=1)(=[O:26])=[O:27]

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 44674964-isothiocyanato-N-1,3-thiazol-2-ylbenzenesulfonamideHCID 43237029HCID 43237029, Verbindung

Produkt 1

HCID 57551211HCID 57551211, VerbindungAusbeute 20 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A mixture of (4-trifluoromethyl-phenyl)-acetic acid hydrazide (55 mg, 0.25 mmol, 1.5 equiv), 4-isothiocyanato-N-thiazol-2-yl-benzenesulfonamide (50 mg, 0.2 mmol, 1.0 equiv) and sodium carbonate (20 mg, 0.18 mmol, 1.1 equiv) in 1.0 mL of ethanol was heated at 85° C. After 16 h, the heterogeneous reaction mixture was concentrated in vacuo, diluted with 500 μL of acetonitrile, filtered, and purified via reverse phase HPLC. The fraction containing product was lyophilized to afford the product as an off-white solid (15 mg, 20%).

Aufarbeitung

  1. concentrationthe heterogeneous reaction mixture was concentrated in vacuo
  2. additiondiluted with 500 μL of acetonitrile
  3. filtrationfiltered
  4. custompurified via reverse phase HPLC
  5. additionThe fraction containing product

Quellen und Nachweise

ORD-Eintrag
ord-2fdb93d8572e4a72b3617c5d02932de3
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08124610B2

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