HCID 12877066、化合物 → 74852-82-7

HRID 1164226ノート

反応式

HRID 1164226 の反応式
[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

参加物

4

反応物 1

HCID 12877066HCID 12877066、化合物

生成物 1

HCID 1287706874852-82-7収率 47%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-000661adac584a59bc7b6acd19fd325d
出典データセット
uspto-grants-1983_01
特許番号
US04368200

反応ノート

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