HCID 12877066, 화합물 → 74852-82-7

HRID 1154736노트

반응식

HRID 1154736 반응식
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[N:5]=[C:4](SC)[N:3]=1>[Ni].CO>[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][N:3]=1

참가 물질

4

반응물 1

HCID 12877066HCID 12877066, 화합물

생성물 1

HCID 1287706874852-82-7수율 47%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

A mixture of 20 parts of 4-[5-methyl-3-(methylthio)-1H-1,2,4-triazol-1-yl]benzenamine, 15 parts of Raney-nickel catalyst and 400 parts of methanol is stirred and refluxed for 2 hours. The Raney-nickel is filtered off and another 15 parts of the catalyst are added. Stirring at reflux is continued for 4 hours. The reaction mixture is filtered, washed on the filter with methanol and the filtrate is evaporated. The residue is crystallized from a mixture of 4-methyl-2-pentanone, 2,2'-oxybispropane and petroleumether. The product is filtered off and dried, yielding 7.6 parts (47%) of 4-(5-methyl-1H-1,2,4-triazol-1-yl)benzenamine; mp. 145° C.

후처리

  1. temperaturerefluxed for 2 hours
  2. filtrationThe Raney-nickel is filtered off
  3. additionanother 15 parts of the catalyst are added
  4. stirringStirring
  5. temperatureat reflux
  6. filtrationThe reaction mixture is filtered
  7. washwashed on the
  8. filtrationfilter with methanol
  9. customthe filtrate is evaporated
  10. customThe residue is crystallized from a mixture of 4-methyl-2-pentanone, 2,2'-oxybispropane and petroleumether
  11. filtrationThe product is filtered off
  12. customdried

출처 및 근거

ORD 기록
ord-a2eee97010ff4746bc3198b73ac267fe
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490530

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