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Acetyl chloride → HCID 57940700、化合物

HRID 1437308
ノート
印刷プレビュー

反応式

HRID 1437308 の反応式
C(N(CC)CC)C.[C:8](Cl)(=[O:10])[CH3:9].[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([N:20]2[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)=[CH:23][C:22]([C:31]([N:33]3[CH2:38][CH2:37][CH2:36][CH2:35][NH:34]3)=[O:32])=[N:21]2)=[CH:16][CH:15]=1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([N:20]2[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)=[CH:23][C:22]([C:31]([N:33]3[CH2:38][CH2:37][CH2:36][CH2:35][N:34]3[C:8](=[O:10])[CH3:9])=[O:32])=[N:21]2)=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 11674985HCID 11674985、化合物

生成物 1

HCID 57940700HCID 57940700、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (0.210 mL), acetyl chloride (0.0807 mL) and 4-dimethylaminopyridine (13.5 mg) were added to 1-[1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)pyrazole-3-carbonyl]hexahydropyridazine (0.275 g) obtained in Example 162 in methylene chloride (6.0 mL) at room temperature, followed by stirring for 20 minutes. The mixture was partitioned between water and chloroform. The organic layer was washed with saturated brine, and then dried over sodium sulfate anhydrate. The mixture was subjected to filtration, and the solvent was removed under reduced pressure. The residue was purified through silica gel column chromatography (chloroform-methanol), to thereby give the title compound as an amorphous product (0.149 g, 59%).

後処理

  1. customThe mixture was partitioned between water and chloroform
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over sodium sulfate anhydrate
  4. filtrationThe mixture was subjected to filtration
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified through silica gel column chromatography (chloroform-methanol)

出典と根拠

ORDレコード
ord-8a17b77d638f45a3a1b6f6114b955e90
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622471B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート