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Water → (4-Methoxy-6-trifluoromethylpyrimidin-5-yl)-methanol

HRID 1172131
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HRID 1172131 반응식
[BH4-].[Na+].[CH3:3][O:4][C:5]1[C:10]([CH:11]=[O:12])=[C:9]([C:13]([F:16])([F:15])[F:14])[N:8]=[CH:7][N:6]=1.O>CO>[CH3:3][O:4][C:5]1[C:10]([CH2:11][OH:12])=[C:9]([C:13]([F:15])([F:14])[F:16])[N:8]=[CH:7][N:6]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 178628984-Methoxy-6-trifluoromethyl-pyrimidine-5-carbaldehyde

생성물 1

HCID 17862874(4-Methoxy-6-trifluoromethylpyrimidin-5-yl)-methanol수율 32.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.24 g (6.3 mmoles) of sodium borohydride was gradually added, at room temperature, to a solution of 1.3 g (6.3 mmoles) of 4-methoxy-6-trifluoromethylpyrimidine-5-carboaldehyde dissolved in 30 ml of methanol. The mixture was stirred for 3 hours to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 0.42 g (yield: 32.1%) of (4-methoxy-6-trifluoromethylpyrimidin-5-yl)-methanol 1H-NMR [CDCl3/TMS, δ (ppm)]:

후처리

  1. customto give rise
  2. customto a reaction
  3. customAfter confirmation of the completion of the reaction
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe resulting organic layer was washed with water
  6. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  7. distillationThe resulting solution was subjected to vacuum distillation
  8. customto remove the solvent
  9. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-7f93744eaae048289c44967118ec3521
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07833939B2

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