1-Bromo-2,4-dimethoxybenzene → HCID 17968171, 화합물

HRID 271571

반응식

HRID 271571 반응식
[Mg].Br[C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][C:4]=1[O:11][CH3:12].Cl.Br[C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1>C1COCC1>[CH3:12][O:11][C:4]1[CH:5]=[C:6]([O:9][CH3:10])[CH:7]=[CH:8][C:3]=1[C:15]1[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 872661-Bromo-2,4-dimethoxybenzeneHCID 881004-Bromopyridinium chlorideHCID 5462224Magnesium

생성물 1

HCID 17968171HCID 17968171, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The Grignard reagent, prepared from magnesium (5 g) and 1-Bromo-2,4-dimethoxybenzene (38 g) in THF (300 ml), is added at room temperature to 4-Bromo-pyridine hydrochloride salt in THF (10 ml). The mixture is heated under reflux for 2 hours and then evaporated to dryness. The residue is taken up in ethyl acetate and extracted with 1N hydrochloric acid. The aqueous phase is neutralised with 4M sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried with magnesium sulfate, evaporated and the residue is purified by column chromatography on silica gel using n-hexane:AcOEt=1:1 (v/v). MS-APCI+ (M+H)+=216

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 2 hours
  3. customevaporated to dryness
  4. extractionextracted with 1N hydrochloric acid
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic phase is dried with magnesium sulfate
  7. customevaporated
  8. customthe residue is purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-5fa6046640ef4ac79636829ba2fcab2e
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452886B2

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