Pyridazine, 3-chloro-, 2-oxide → HCID 178420148、化合物

HRID 2096354ノート

反応式

HRID 2096354 の反応式
[C:1]1([C:7]2[N:12]=[CH:11][C:10]([C:13]3[N:14]=[C:15]([CH:18]4[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]4)[NH:16][CH:17]=3)=[CH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:25]1[N+:30]([O-])=[N:29][CH:28]=[CH:27][CH:26]=1>CS(C)=O.O>[C:1]1([C:7]2[N:12]=[CH:11][C:10]([C:13]3[N:14]=[C:15]([CH:18]4[CH2:23][CH2:22][N:21]([C:28]5[N:29]=[N:30][CH:25]=[CH:26][CH:27]=5)[CH2:20][CH2:19]4)[NH:16][CH:17]=3)=[CH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 2

HCID 6403197Pyridazine, 3-chloro-, 2-oxideHCID 178420149HCID 178420149、化合物

生成物 1

HCID 178420148HCID 178420148、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

The title compound is prepared in a similar manner described above using Buchwald-Hartwig amination conditions or as described in PCT International Application 2006/058338, 1 Jun. 2006. In this case, a solution consisting of 2-phenyl-5-(2-(piperidin-4-yl)-1H-imidazol-4-yl)pyrimidine and 6-chloropyridazine 1-oxide (preparation of this reagent can be found in PCT International Application 2007/106670, 20 Sep. 2007 and Chemical and Pharmaceutical Bulletin, 1963, 11, 261-263) in dimethylsulfoxide is heated at 80° C. for 18 hours. The reaction mixture is cooled, diluted with water and the organic material is extracted with ethyl acetate. The organic phase is washed with brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue is chromatographed on silica to afford the title compound.

後処理

  1. customThe title compound is prepared in a similar manner
  2. custompreparation of this reagent
  3. temperatureThe reaction mixture is cooled
  4. extractionthe organic material is extracted with ethyl acetate
  5. washThe organic phase is washed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue is chromatographed on silica

出典と根拠

ORDレコード
ord-9382503c6fd64d23bd33a72cf119a74e
出典データセット
uspto-grants-2013_05
特許番号
US08450326B2

反応ノート

読み込み中…