반응 #1050852

반응 방정식

4-chloro-2-methyl-2H-indazole

n-butyl lithium

sulfurous acid

→

lithium 4-chloro-2-methyl-2H-indazole-3-sulfinate

용매

ethyl ether

ethyl ether

반응 조건

후처리

1. 1
   workup.WAITat a temperature of not higher than -20° C. for 3 hours
2. 2
   기타After completion of the reaction
3. 3
   기타was returned to room temperature
4. 4
   여과the product was subjected to filtration
5. 5
   기타Crystals were dried

실험 절차

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.

출처