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Water → (2-Bromo-3-methylphenyl)(pyrimidin-4-yl)methanol

HRID 1028977
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반응식

HRID 1028977 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]([C:11]1[CH:16]=[CH:15][N:14]=[C:13](SC)[N:12]=1)=[O:10].O>CCO.[Ni]>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]([C:11]1[CH:16]=[CH:15][N:14]=[CH:13][N:12]=1)[OH:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 962WaterHCID 67325293(2-Bromo-3-methylphenyl)(2-(methylthio)pyrimidin-4-yl)methanone

생성물 1

HCID 67324212(2-Bromo-3-methylphenyl)(pyrimidin-4-yl)methanol

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

To a solution of (2-bromo-3-methylphenyl)(2-(methylthio)pyrimidin-4-yl)methanone (0.10 g, 0.309 mmol) in EtOH (10 mL) was added Raney 2800 nickel, slurry, in water (0.022 mL, 3.41 mmol) and the resulting mixture was reflux until starting material was consumed (2 h). The mixture was brought to RT and decanted. The remaining Ni was extracted with DCM/NH3 (2M in MeOH). The combined organic layers were concentrated and the residue obtained was extracted with DCM and the extracts were combined and concentrated to afford a yellow oil as (2-bromo-3-methylphenyl)(pyrimidin-4-yl)methanol which was used without purification.

후처리

  1. customwas consumed (2 h)
  2. customwas brought to RT
  3. customdecanted
  4. extractionThe remaining Ni was extracted with DCM/NH3 (2M in MeOH)
  5. concentrationThe combined organic layers were concentrated
  6. customthe residue obtained
  7. extractionwas extracted with DCM
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fa29cff280524d65a83d6afcfc645056
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735384B2

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