6-Nitroindazole → HCID 178526457, Verbindung

HRID 1163379

Reaktionsgleichung

Reaktionsgleichung von HRID 1163379
[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].S(Cl)([Cl:16])(=O)=O>ClCCCl>[Cl:16][C:8]1[C:7]2[C:11](=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[NH:10][N:9]=1

Komponenten

4

Edukt 2

HCID 242396-NitroindazoleHCID 24648Sulfuryl chloride

Produkt 1

HCID 178526457HCID 178526457, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 6-nitroindazole (2 mmol) in DCE (5 mL), sulfuryl chloride (10 mmol) was added and the resulting mixture was heated 80° C. for 3-5 h. The reaction mixture was concentrated, added with 5% aqueous Na2CO3 solution (20 mL) and extracted with EtOAc (2×15 mL). The combined organics were then washed with water (20 mL) and brine (20 mL) and dried over anhydrous Na2SO4. Removal of volatiles afforded 3-chloro-6-nitro-1H-indazole as a yellow solid.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. additionadded with 5% aqueous Na2CO3 solution (20 mL)
  3. extractionextracted with EtOAc (2×15 mL)
  4. washThe combined organics were then washed with water (20 mL) and brine (20 mL)
  5. dry with materialdried over anhydrous Na2SO4
  6. customRemoval of volatiles

Quellen und Nachweise

ORD-Eintrag
ord-7bbb058a81d34b68b4e884d71d30497d
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820821B2

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