Water → 6-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

HRID 397573

反応式

HRID 397573 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.Cl[C:13]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(C(C)C)C(C)C)C.O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[N:9]([C:13]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)([C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[N:10]=2)[N:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6456Trityl chlorideHCID 81531DiisopropylethylamineHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

生成物 1

HCID 230003076-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one収率 71.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.341 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one and 0.669 g of chlorotriphenylmethane were dissolved in 5 ml of N,N-dimethylformamide; 0.414 ml of N-ethyldiisopropylamine was added, followed by stirring at room temperature for 2 days. After water was added, the reaction mixture was extracted with ethyl acetate; the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (2:1). The desired fraction was collected and concentrated; the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.591 g of the title compound.

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washthe extract was washed with saline
  3. dry with materialdried over magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. washeluted with hexane-ethyl acetate (2:1)
  6. customThe desired fraction was collected
  7. concentrationconcentrated
  8. customthe crystal obtained
  9. filtrationwas collected by filtration
  10. washwashed with diethyl ether
  11. customdried

出典と根拠

ORDレコード
ord-fbbef0e461ac4f1bafb5463b640ff18f
出典データセット
uspto-grants-2003_08
特許番号
US06610694B1

関連ノート

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