Potassium Carbonate → HCID 54579446、化合物

HRID 75482ノート

反応式

HRID 75482 の反応式
Cl.[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.Br[CH2:17][CH2:18][CH2:19][N:20]1[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]2[C:21]1=[O:30].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:15][CH2:14][N:13]([CH2:17][CH2:18][CH2:19][N:20]2[C:24](=[O:25])[C:23]3[C:22](=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:21]2=[O:30])[CH2:12][CH2:11]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 21611N-3-Bromopropylphthalimide2 回HCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride2 回

生成物 1

HCID 54579446HCID 54579446、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The mixture of 1-(2,3-dichlorophenyl)piperazine hydrochloride (compound 35, 10.0 g, 37.4 mmol), N-(3-bromopropyl)phthalimide (compound 34, 9.09 g, 33.9 mmol) and potassium carbonate (11.7 g, 84.8 mmol) in DMF was stirred at room temperature. The mixture was concentrated under reduced pressure. The residue was diluted with CH2Cl2, and washed with water. The organic layer was dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The obtained product was washed with EtOH to provide the title compound (11.2 g, 80%) as a white solid.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionThe residue was diluted with CH2Cl2
  3. washwashed with water
  4. dry with materialThe organic layer was dried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. washThe obtained product was washed with EtOH

出典と根拠

ORDレコード
ord-cd309cc602ba4572a91bf3835eed1698
出典データセット
uspto-grants-2014_09
特許番号
US08835436B2

反応ノート

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