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Ammonium formate → 2-Hydroxy-4-pyrazol-1-yl-benzonitrile

HRID 1271519
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HRID 1271519 반응식
C([O:8][C:9]1[CH:16]=[C:15]([N:17]2[CH:21]=[CH:20][CH:19]=[N:18]2)[CH:14]=[CH:13][C:10]=1[C:11]#[N:12])C1C=CC=CC=1.C([O-])=O.[NH4+]>C1COCC1.[Pd]>[OH:8][C:9]1[CH:16]=[C:15]([N:17]2[CH:21]=[CH:20][CH:19]=[N:18]2)[CH:14]=[CH:13][C:10]=1[C:11]#[N:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 184528912-Benzyloxy-4-pyrazol-1-yl-benzonitrile

생성물 1

HCID 223926322-Hydroxy-4-pyrazol-1-yl-benzonitrile수율 57.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C
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실험 절차

To 0.395 g of the material from Step B, above, dissolved in 10 mL THF, is added a catalytic amount of 10% Pd/C and excess ammonium formate. The reaction is heated to 50° C. for 45 minutes. Upon cooling, celite is added. The reaction is then gravity filtered and concentrated in vacuo. The residue is redissolved in ethyl acetate and washed with water, brine, dried over sodium sulfate, filtered and concentrated in vacuo to give 0.152 g of the final title compound (57.1%).

후처리

  1. temperatureUpon cooling
  2. additioncelite is added
  3. filtrationgravity filtered
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue is redissolved in ethyl acetate
  6. washwashed with water, brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-112fafd45f344dbfb7153c7b8e378b06
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07205313B2

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