Sulfurous Acid → HCID 23675696, Verbindung

HRID 1378935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1378935
[Cl:1][C:2]1[C:3]2[C:7]([CH:8]=[CH:9][CH:10]=1)=[N:6][N:5]([CH3:11])[CH:4]=2.C([Li:16])CCC.[S:17](=O)([OH:19])[OH:18]>C(OCC)C>[Cl:1][C:2]1[C:3]2[C:7]([CH:8]=[CH:9][CH:10]=1)=[N:6][N:5]([CH3:11])[C:4]=2[S:17]([O-:19])=[O:18].[Li+:16]

Komponenten

5

Edukt 3

HCID 1100Sulfurous AcidHCID 190831754-Chloro-2-methyl-2H-indazoleHCID 178418339Butyllithium

Produkt 1

HCID 23675696HCID 23675696, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
-30 °C

Versuchsvorschrift

A solution containing 16 g (0.1 mol) of 4-chloro-2-methyl-2H-indazole in 300 ml of ethyl ether, was cooled to -30° C., and 85.4 g (0.2 mol) of n-butyl lithium (15% hexane solution) was dropwise added thereto. The mixture was stirred for one hour at the same temperature. Then, an excess amount of sulfurous acid gas was blown thereinto at a temperature of not higher than -20° C. for 3 hours. After completion of the reaction, the mixture was returned to room temperature and diluted with ethyl ether, and the product was subjected to filtration. Crystals were dried to obtain crude lithium 4-chloro-2-methyl-2H-indazole-3-sulfinate. This product was used for the subsequent reaction without purification.

Aufarbeitung

  1. waitat a temperature of not higher than -20° C. for 3 hours
  2. customAfter completion of the reaction
  3. customwas returned to room temperature
  4. filtrationthe product was subjected to filtration
  5. customCrystals were dried

Quellen und Nachweise

ORD-Eintrag
ord-99b3e4c3adbb4f988bae7c1bd2c23ce4
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05670452

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