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Water → HCID 69692723、化合物

HRID 1635930
ノート
印刷プレビュー

反応式

HRID 1635930 の反応式
[NH2:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=2)=[C:5]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[N:4]([CH3:20])[N:3]=1.C(N(CC)CC)C.[C:28]1([CH2:34][C:35](Cl)=[O:36])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.O>O1CCCC1>[F:19][C:16]1[CH:17]=[CH:18][C:13]([C:5]2[N:4]([CH3:20])[N:3]=[C:2]([NH:1][C:35](=[O:36])[CH2:34][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:6]=2[C:7]2[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=2)=[CH:14][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 4

HCID 962WaterHCID 7679Phenylacetyl chlorideHCID 8471TriethylamineHCID 18674082HCID 18674082、化合物

生成物 1

HCID 69692723HCID 69692723、化合物収率 64%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

338 mg of 3-amino-5-(4-fluorophenyl)-1-methyl-4-(4-pyridyl)pyrazole was dissolved in 20 ml of a tetrahydrofuran, followed by the addition of 140 mg of triethylamine. Then, 5 ml of a tetrahydrofuran solution containing 214 mg of phenylacetyl chloride was added dropwise thereto, followed by stirring at room temperature overnight. After the addition of water, the reaction mixture was extracted with chloroform. After the organic layer was washed with water and dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography using 80 g of silica gel [with an elution solvent comprising chloroform-methanol (40:1)]. Thus, 310 mg (64% yield) of the title compound was obtained as pale-yellow crystals.

後処理

  1. additionwas added dropwise
  2. extractionthe reaction mixture was extracted with chloroform
  3. washAfter the organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe resulting residue was purified by column chromatography

出典と根拠

ORDレコード
ord-0c13352279af45d5b19752b24102cb06
出典データセット
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06511997B1

反応ノート

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