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1-Bromo-2,2-dimethylpropane → HCID 58612135, 화합물

HRID 1049464
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HRID 1049464 반응식
Br[CH2:2][C:3]([CH3:6])([CH3:5])[CH3:4].[Mg].Br[C:9]1[C:10]([O:15][CH3:16])=[N:11][CH:12]=[CH:13][CH:14]=1.[Cl-].[NH4+]>C(OCC)C.C1COCC1.CC(C1C=CC=C(C(C)C)C=1N1[C-]=[N+](C2C(C(C)C)=CC=CC=2C(C)C)CC1)C>[CH3:16][O:15][C:10]1[C:9]([CH2:2][C:3]([CH3:6])([CH3:5])[CH3:4])=[CH:14][CH:13]=[CH:12][N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 124151-Bromo-2,2-dimethylpropaneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 125333903-Bromo-2-methoxypyridine

생성물 1

HCID 58612135HCID 58612135, 화합물

시약·촉매·용매 3

HCID 10883669SIPr촉매
HCID 3283
Diethyl Ether
용매
HCID 8028Tetrahydrofuran용매

실험 절차

Under an argon atmosphere, a solution of 1-bromo-2,2-dimethylpropane (14.8 mL) in diethyl ether (120 mL) was added dropwise to magnesium (3.15 g) at a slow refluxing rate. The reaction mixture was heated under reflux for 30 min, and the obtained solution was added dropwise to a solution of 3-bromo-2-methoxypyridine (4.43 g) and PEPPSI™-SIPr (trade name) (805 mg) in THF (80 mL) at room temperature. The reaction mixture was stirred at room temperature for 30 min, and saturated aqueous ammonium chloride solution was added at room temperature. The reaction mixture was extracted with ethyl acetate, and the extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give a crude product of the title compound (4.24 g) as a pale-yellow oil. This compound was used for the next step without further purification.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 30 min
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. washthe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-276c3ac8f3554b84a035083cd4b108c5
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382188B2

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