반응 #449845

반응 방정식

3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole

sodium hydrogen phosphate

→

3-Amino-1-methyl-5-methylmercaptopyrazole

용매

caustic soda

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled
2. 2
   추출extracted with ethyl acetate
3. 3
   건조The organic phase was dried over sodium sulfate
4. 4
   농축concentrated
5. 5
   기타the residue purified by silica gel chromatography (hexane/ethyl acetate 1:1)

실험 절차

5.55 g (33.0 mmol) 3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole heated with 50 ml 32% caustic soda at boiling for 24 hours. The reaction mixture was cooled, made slightly acidic with aqueous sodium hydrogen phosphate, heated for 8 hours at 50° C. and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, concentrated and the residue purified by silica gel chromatography (hexane/ethyl acetate 1:1).

출처