Potassium Carbonate → 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one

HRID 1947637

반응식

HRID 1947637 반응식
F[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[NH:7][CH2:6][CH2:5]2.[C:13](=[O:16])([O-])[O-].[K+].[K+]>C(N)C1C=CC=CC=1>[CH2:8]([NH:7][C:6]1[CH:5]=[C:4]2[C:3](=[CH:2][CH:11]=1)[C:13](=[O:16])[NH:7][CH2:6][CH2:5]2)[C:9]1[CH:10]=[CH:11][CH:2]=[CH:3][CH:4]=1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 107257096-Fluoro-1,2,3,4-tetrahydroisoquinolin-1-one

생성물 1

HCID 672239156-benzylamino-3,4-dihydro-2H-isoquinolin-1-one수율 35%

시약·촉매·용매 1

HCID 7504Benzylamine용매

실험 절차

A solution of 6-fluoro-3,4-dihydro-2H-isoquinolin-1-one (300 mg, 1.81 mmol) and potassium carbonate (550 mg, 3.98 mmol) in benzylamine (1.5 ml) was stirred at 180° C. in a microwave for 2 hrs. The solvent was evaporated and the resulting residue partitioned between ethyl acetate (10 ml) and water (10 ml). The organic phase was separated, washed with brine (10 ml), then dried (MgSO4) and evaporated in vacuo. The crude residue was purified by preparative HPLC (Method A) to yield the title compound as a colourless solid (80 mg, 18%). HPLC retention time 3.81 min. Mass spectrum (ES+) m/z 253 (M+H).

후처리

  1. customThe solvent was evaporated
  2. customthe resulting residue partitioned between ethyl acetate (10 ml) and water (10 ml)
  3. customThe organic phase was separated
  4. washwashed with brine (10 ml)
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo
  7. customThe crude residue was purified by preparative HPLC (Method A)

출처 및 근거

ORD 기록
ord-fa7e5e71fe5642d8a90aa87b2e5ae477
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399481B2

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