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

HRID 1945726

반응식

HRID 1945726 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)
  5. dry with materialThe combined DCM solutions were dried (Na2SO4)
  6. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-4ac34d4c131d4132895ea6819fd19128
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394796B2

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