반응 #1909

반응 방정식

product

3-cyano-4-trifluoromethylsulfenyl-5-(N-trifluoroacetylamino)pyrazole

ammonium hydroxide

hydrochloric acid

→

title compound

수율 87.6%

3-cyano-4-trifluoromethylsulfenyl-5-aminopyrazole

수율 87.6%

용매

methanol

ethyl acetate

반응 조건

후처리

1. 1
   온도the solution was refluxed for 3 hours
2. 2
   세척The organic layer was washed several times with water and brine
3. 3
   건조dried over MgSO4
4. 4
   농축concentrated to dryness
5. 5
   기타to give an oily brown residue which
6. 6
   기타was recrystallized from methyl tert-butyl ether

실험 절차

The product of Step E (55 g, 181 mmoles) was dissolved in methanol. 100 ml of ammonium hydroxide were added, the solution was refluxed for 3 hours and then stirred at room temperature for 15 hours. The methanolic solution was brought to pH7 using concentrated aqueous hydrochloric acid and diluted with ethyl acetate. The organic layer was washed several times with water and brine, dried over MgSO4 and concentrated to dryness to give an oily brown residue which was recrystallized from methyl tert-butyl ether to afford 33 g of the title compound, m.p. around 187° C.

출처