Methanol → 4-bromo-N-ethylisoquinolin-1-amine

HRID 1922899

반응식

HRID 1922899 반응식
[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](Cl)=[N:4][CH:3]=1.CO.[CH2:15]([NH2:17])[CH3:16]>>[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([NH:17][CH2:15][CH3:16])=[N:4][CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 6341EthylamineHCID 4597664-Bromo-1-chloroisoquinoline

생성물 1

HCID 596052034-bromo-N-ethylisoquinolin-1-amine수율 88%

반응 조건

온도
50 °C

실험 절차

To a suspension of 4-bromo-1 chloroisoquinoline (0.831 g, 3.43 mmol) in MeOH (10.3 mL, 254 mmol) was added ethylamine (70% in water, 1.1 mL). The mixture was heated at 50° C. for 16 h. The mixture was concentrated. The residue was partitioned between water (20 mL) and DCM (20 mL). DCM layer was separated. The aqueous layer was extracted with DCM (10 mL) The combined DCM solutions were dried (Na2SO4). Filtration and concentration gave 4-bromo-N-ethylisoquinolin-1-amine (0.761 g, 88%). LCMS: M+H+=251.

후처리

  1. concentrationThe mixture was concentrated
  2. customThe residue was partitioned between water (20 mL) and DCM (20 mL)
  3. customDCM layer was separated
  4. extractionThe aqueous layer was extracted with DCM (10 mL) The combined DCM solutions
  5. dry with materialwere dried (Na2SO4)
  6. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-ac312d68479d428696847172550e0583
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173650B2

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