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1-Bromo-2,2-dimethylpropane → 3-(2-Fluoro-5-methoxyphenyl)-6-methoxy-2-neopentylpyridine

HRID 1049391
ノート
印刷プレビュー

反応式

HRID 1049391 の反応式
Br[CH2:2][C:3]([CH3:6])([CH3:5])[CH3:4].[Mg].Cl[C:9]1[C:14]([C:15]2[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:16]=2[F:23])=[CH:13][CH:12]=[C:11]([O:24][CH3:25])[N:10]=1.[Cl-].[NH4+]>C(OCC)C.CC(C1C=CC=C(C(C)C)C=1N1[C-]=[N+](C2C(C(C)C)=CC=CC=2C(C)C)CC1)C.C1COCC1>[F:23][C:16]1[CH:17]=[CH:18][C:19]([O:21][CH3:22])=[CH:20][C:15]=1[C:14]1[C:9]([CH2:2][C:3]([CH3:6])([CH3:5])[CH3:4])=[N:10][C:11]([O:24][CH3:25])=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 124151-Bromo-2,2-dimethylpropaneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 1177600232-Chloro-3-(2-fluoro-5-methoxyphenyl)-6-methoxypyridine

生成物 1

HCID 1177601343-(2-Fluoro-5-methoxyphenyl)-6-methoxy-2-neopentylpyridine

試薬・触媒・溶媒 3

HCID 10883669
SIPr
触媒
HCID 3283Diethyl Ether溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

Under an argon atmosphere, a solution of 1-bromo-2,2-dimethylpropane (9.82 mL) in diethyl ether (100 mL) was added dropwise to magnesium (1.72 g) at a slow refluxing rate, and the reaction mixture was heated under reflux further for 1 hr. Under an argon atmosphere, the obtained solution was added dropwise to a solution of 2-chloro-3-(2-fluoro-5-methoxyphenyl)-6-methoxypyridine (3.79 g) and a PEPPSI™-SIPr catalyst (trade name) (970 mg) in THF (70 mL) at room temperature, and the mixture was stirred at room temperature for 15 min. To the reaction mixture was added saturated aqueous ammonium chloride solution at room temperature, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (3.97 g) as a colorless oil.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux further for 1 hr
  3. extractionthe 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
  7. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-f55c46a76d934468a25155967e9e418f
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382188B2

反応ノート

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