Triethylamine → 3-[4-(3-Methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazine

HRID 486458ノート

反応式

HRID 486458 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[CH:6][CH:7]=1.[CH3:12][C:13]1[CH:14]=[C:15]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[CH:16]=[CH:17][CH:18]=1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:12][C:13]1[CH:14]=[C:15]([N:19]2[CH2:24][CH2:23][N:22]([C:2]3[N:3]=[N:4][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[CH:6][CH:7]=3)[CH2:21][CH2:20]2)[CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 831111-(m-Tolyl)piperazineHCID 2524763-Chloro-6-(methylsulfonyl)pyridazine

生成物 1

HCID 151246013-[4-(3-Methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazine収率 89%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 3.2 parts of 3-chloro-6-(methylsulfonyl)pyridazine, 3 parts of 1-(3-methylphenyl)piperazine, 2 parts of N,N-diethylethanamine and 180 parts of benzene was stirred for 24 hours at reflux. The reaction mixture was evaporated. Water was added to the residue. The precipitated product was filtered off, washed with water and dissolved in trichloromethane. The solution was dried, filtered and evaporated. The residue was crystallized from methanol. The product was filtered off and dried, yielding 5 parts (89%) of 3-[4-(3-methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazine; mp. 201° C. (compound 209).

後処理

  1. temperatureat reflux
  2. customThe reaction mixture was evaporated
  3. additionWater was added to the residue
  4. filtrationThe precipitated product was filtered off
  5. washwashed with water
  6. dissolutiondissolved in trichloromethane
  7. customThe solution was dried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue was crystallized from methanol
  11. filtrationThe product was filtered off
  12. customdried

出典と根拠

ORDレコード
ord-a30fdb6e4d7848be80154ba15f0f3aaa
出典データセット
uspto-grants-1994_03
特許番号
US05292738

反応ノート

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