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

HRID 1947637

反応式

HRID 1947637 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 7504Benzylamine溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-fa7e5e71fe5642d8a90aa87b2e5ae477
出典データセット
uspto-grants-2013_03
特許番号
US08399481B2

関連ノート

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