1-Phenylpiperazine → 2-[3-(4-Phenyl-piperazin-1-yl)-propyl]-isoindole-1,3-dione

HRID 1284629ノート

反応式

HRID 1284629 の反応式
Br[CH2:2][CH2:3][CH2:4][N:5]1[C:9](=[O:10])[C:8]2=[CH:11][CH:12]=[CH:13][CH:14]=[C:7]2[C:6]1=[O:15].[C:16]1([N:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:16]1([N:22]2[CH2:27][CH2:26][N:25]([CH2:2][CH2:3][CH2:4][N:5]3[C:9](=[O:10])[C:8]4=[CH:11][CH:12]=[CH:13][CH:14]=[C:7]4[C:6]3=[O:15])[CH2:24][CH2:23]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 3

HCID 70961-PhenylpiperazineHCID 11430Potassium CarbonateHCID 21611N-3-Bromopropylphthalimide

生成物 1

HCID 64248092-[3-(4-Phenyl-piperazin-1-yl)-propyl]-isoindole-1,3-dione収率 90%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To the solution of N-(3-bromopropyl)phthalimide (15.6 g) in acetone (150 ml) were added 1-phenylpiperazine (10.4 g) and potassium carbonate (12.0 g). The resulting mixture was refluxed with stirring for 4.5 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with acetone. The filtrate and washing were combined and evaporated under reduced pressure. The residue was recrystallized from ethanol to give an oil of N-[3-(4-phenyl-1-piperazinyl)propyl]phthalimide (18.3 g), mp 129° to 134° C.

後処理

  1. temperatureThe resulting mixture was refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. washThe filter cake was washed with acetone
  5. washThe filtrate and washing
  6. customevaporated under reduced pressure
  7. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-4e6c4edf18264675b7f9d656e5be5178
出典データセット
uspto-grants-1986_01
特許番号
US04563524

反応ノート

読み込み中…