Reaktion #354225

Reaktionsgleichung

1-benzenesulfonyl-3-(1-methyl-4-piperazinyl)-1H-indazole

phenyl chloroformate

→

white solid

Ausbeute 55.1%

1-Benzenesulfonyl-3-(1-phenoxycarbonyl-4-piperazinyl)-1H-indazole

Ausbeute 55.1%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was warmed
2. 2
   Temperaturto reflux for 2 hours
3. 3
   Einengenconcentrated
4. 4
   workup.ADDITIONThe residue was diluted with ethyl acetate
5. 5
   Filtrationfiltered
6. 6
   Sonstigepurified via flash column chromatography (silica gel, ethyl acetate)
7. 7
   workup.ADDITIONConcentration of the product containing fractions
8. 8
   Sonstigegave an oil which
9. 9
   WaschenThe product was washed well with heptane

Vorschrift

To a solution of 1-benzenesulfonyl-3-(1-methyl-4-piperazinyl)-1H-indazole (2.1 g, 5.89 mmol) in dichloromethane (100 ml) was added phenyl chloroformate (3.8 ml, 29.45 mmol) at room temperature. The reaction mixture was warmed to reflux for 2 hours, cooled to room temperature, and concentrated. The residue was diluted with ethyl acetate, filtered and purified via flash column chromatography (silica gel, ethyl acetate). Concentration of the product containing fractions gave an oil which solidified on standing. The product was washed well with heptane to give 1.5 g of a white solid, m.p. 112°-114° C.

Quelle