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Water → HCID 68469062, 화합물

HRID 503018
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HRID 503018 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 68469380HCID 68469380, 화합물

생성물 1

HCID 68469062HCID 68469062, 화합물수율 71.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-88b9e96f921e4f64b3175855fb46040d
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776897B2

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