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Sodium borohydride → [1-methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazol-4-yl]-methanol

HRID 1192945
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HRID 1192945 반응식
[CH3:1][N:2]1[C:6]([O:7][CH:8]2[CH2:11][O:10][CH2:9]2)=[C:5]([CH:12]=[O:13])[C:4]([C:14]([F:17])([F:16])[F:15])=[N:3]1.[BH4-].[Na+]>CO>[CH3:1][N:2]1[C:6]([O:7][CH:8]2[CH2:11][O:10][CH2:9]2)=[C:5]([CH2:12][OH:13])[C:4]([C:14]([F:17])([F:15])[F:16])=[N:3]1
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 597395451-methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazole-4-carbaldehyde

생성물 1

HCID 59739609[1-methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazol-4-yl]-methanol수율 69.6%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

1-Methyl-5-(oxetan-3-yloxy)-3-trifluoromethyl-1H-pyrazole-4-carbaldehyde (11.6 g, 46.4 mmol) was dissolved in methanol (100 ml) and sodium borohydride (0.87 g, 23.0 mmol) was added in portions at 0° C. After stirring at 0° C. for 2 hours the mixture was concentrated and the oil was dissolved in dichloromethane (100 ml). The solution was washed with water and brine, dried over magnesium sulfate and concentrated to give the product as yellow solid (8.14 g) which was used in the next step without further purification.

후처리

  1. concentrationwas concentrated
  2. dissolutionthe oil was dissolved in dichloromethane (100 ml)
  3. washThe solution was washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9a1fe51267594677b49c82afc34b9f86
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680290B2

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