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Water → HCID 68469062、化合物

HRID 503018
ノート
印刷プレビュー

反応式

HRID 503018 の反応式
FC(F)(F)C(O)=O.O.[Cl:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[N:20]([CH3:21])[C:19]([C:22]([CH3:35])([CH3:34])[CH:23]([O:30]COC)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[N:18][N:17]=1>C(Cl)Cl>[Cl:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[N:20]([CH3:21])[C:19]([C:22]([CH3:34])([CH3:35])[CH:23]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[OH:30])=[N:18][N:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 68469380HCID 68469380、化合物

生成物 1

HCID 68469062HCID 68469062、化合物収率 71.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (3 ml) and water (1 ml) were added to a methylene chloride (3 ml) solution of 3-(2-chlorophenyl)-5-[2-(methoxymethoxy)-1,1-dimethyl-2-phenylethyl]-4-methyl-4H-1,2,4-triazole (173 mg) under ice cooling, followed by stirring at room temperature for 19 hours. Then, the whole was stirred at 40° C. for 3.5 hours, at 50° C. for 2.5 hours and at 60° C. for 65 hours. The reaction mixture was concentrated under reduced pressure and ethyl acetate and a saturated sodium hydrogen carbonate solution were added thereto. The organic layer was dried over anhydrous sodium sulfate and then the solvent was removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=40:1) to obtain 2-[5-(2-chlorophenyl)-4-methyl-4H-1,2,4-triazol-3-yl]-2-methyl-1-phenylpropan-1-ol (110 mg).

後処理

  1. stirringThen, the whole was stirred at 40° C. for 3.5 hours, at 50° C. for 2.5 hours and at 60° C. for 65 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure and ethyl acetate
  3. additiona saturated sodium hydrogen carbonate solution were added
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was removed by evaporation under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (chloroform:methanol=40:1)

出典と根拠

ORDレコード
ord-88b9e96f921e4f64b3175855fb46040d
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776897B2

反応ノート

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