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Cesium carbonate → HCID 86721065, 화합물

HRID 930901
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HRID 930901 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].Br[CH2:11][CH:12]1[CH2:14][CH2:13]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH2:11][CH:12]1[CH2:14][CH2:13]1
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참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 81503BromomethylcyclopropaneHCID 2650902-Bromo-3-methylphenol

생성물 1

HCID 86721065HCID 86721065, 화합물수율 100.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A 250 mL flask with stirbar was charged with 2-bromo-3-methylphenol (2.86 g, 15.3 mmol), (bromomethyl)cyclopropane (1.80 mL, 18.6 mmol) and cesium carbonate (7.46 g, 22.9 mmol) in dimethylformamide (50 mL). The mixture was stirred for 16 hours at ambient temperature and then heated at 50° C. for 3 hours. The mixture was cooled to ambient temperature and partitioned between ethyl acetate (200 mL) and saturated aqueous sodium chloride (200 mL). The organics were washed twice with saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, filtered, and concentrated to provide the title compound (3.7 g, 100%).

후처리

  1. temperatureheated at 50° C. for 3 hours
  2. temperatureThe mixture was cooled to ambient temperature
  3. custompartitioned between ethyl acetate (200 mL) and saturated aqueous sodium chloride (200 mL)
  4. washThe organics were washed twice with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-51c09e06457549a7a10831618546122f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296741B2

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