Potassium Carbonate → 4-(1-Piperazinyl)isoquinoline

HRID 2227799ノート

反応式

HRID 2227799 の反応式
Cl[CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[C:10](=O)([O-])[O-].[K+].[K+].N1[C:21]2[CH:22]=[CH:23][CH:24]=[N:25][C:20]=2[CH2:19]NC1>CN(C=O)C>[N:4]1([C:3]2[C:22]3[C:23](=[CH:10][CH:19]=[CH:20][CH:21]=3)[CH:24]=[N:25][CH:2]=2)[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 4174751-(2-Chloroethyl)piperazineHCID 66600268Tetrahydropyridopyrimidine

生成物 1

HCID 117698304-(1-Piperazinyl)isoquinoline収率 187.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.9 g (10 mmol) of chloroethylpiperazine and 2.8 g (20 mmol) of potassium carbonate were added to a solution of 2.4 g (10 mmol) of tetrahydropyridopyrimidine in 40 ml of DMF. After reaction at 90° C. for two hours, and then poured onto ice-water and extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution and dried over sodium sulfate, and the solvent was removed under reduced pressure. The oil that remained was taken up in acetone, and the hydrochloride was precipitated out using isopropanol/HCI. This gave 4 g (75%) of the product were obtained (melting point 205° C.).

後処理

  1. customAfter reaction at 90° C. for two hours
  2. additionpoured onto ice-water
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customthe hydrochloride was precipitated out

出典と根拠

ORDレコード
ord-6038d8da371746488e8d1f2b08b8c1e1
出典データセット
uspto-grants-2002_07
特許番号
US06414157B1

反応ノート

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