Reaktion #2446908

Reaktionsgleichung

1-(2,2-difluoroethyl)-3-(2-iodophenyl)-1H-[1,3]thiazolo[4,5-c][1,2]thiazin-4-ol 2,2-dioxide

pyridine

methyl chlorothioformate

→

O-[1-(2,2-difluoroethyl)-3-(2-iodophenyl)-2,2-dioxido-1H-[1,3]thiazolo[4,5-c][1,2]thiazin-4-yl] S-methyl thiocarbonate

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at RT for a further 4 h
2. 2
   SonstigeAfter removing the solvent under reduced pressure
3. 3
   Sonstigethe residue was purified by column chromatography (SiO2, gradient ethyl acetate/n-heptane 10:90 to 75:25)

Vorschrift

150 mg (0.3 mmol) of 1-(2,2-difluoroethyl)-3-(2-iodophenyl)-1H-[1,3]thiazolo[4,5-c][1,2]thiazin-4-ol 2,2-dioxide (compound I-a-14) were dissolved in 5 ml of dichloromethane, and 0.04 ml (0.48 mmol) of pyridine was added at RT. The reaction mixture was stirred at RT for 5 min, and then 0.03 ml (0.38 mmol) of methyl chlorothioformate was added and the mixture was stirred at RT for a further 4 h. After removing the solvent under reduced pressure, the residue was purified by column chromatography (SiO2, gradient ethyl acetate/n-heptane 10:90 to 75:25). This gave 144 mg of compound I-c-16.

Quelle