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Benzyl Bromide → HCID 58764188, 화합물

HRID 2387045
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HRID 2387045 반응식
C(=O)([O-])[O-].[K+].[K+].[CH2:7](Br)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][C:23]([F:26])([F:25])[F:24])[C:17]=1[OH:27]>CN(C=O)C>[CH2:7]([O:27][C:17]1[C:18]([CH2:22][C:23]([F:24])([F:25])[F:26])=[CH:19][CH:20]=[CH:21][C:16]=1[CH3:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 58764013HCID 58764013, 화합물

생성물 1

HCID 58764188HCID 58764188, 화합물수율 108.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium carbonate (953 mg, 6.89 mmol) followed by benzyl bromide (0.8 mL, 6.89 mmol) were added to a solution of 2-methyl-6-(2,2,2-trifluoro-ethyl)-phenol (1.78 g, 6.89 mmol) in DMF (20 mL). The mixture was stirred at room temperature for 15 hours and then partitioned between H2O and EtOAc. The organic layer was washed with 1N HCl, brine, dried over Na2SO4 and concentrated to a brown oil. Purification by flash column chromatography (0% to 20% EtOAc in hexanes) gave the product as a clear oil (2.1 g). LCMS: APCI−VE=279

후처리

  1. custompartitioned between H2O and EtOAc
  2. washThe organic layer was washed with 1N HCl, brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to a brown oil
  5. customPurification by flash column chromatography (0% to 20% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-822b6c6ad17549fabd461dfd43d6f060
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268835B2

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