Sodium Iodide → HCID 21187763、化合物

HRID 1383458ノート

反応式

HRID 1383458 の反応式
Br.[CH:2]([NH:15][CH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Br[CH2:23][CH2:24][N:25]1[C:29](=[O:30])[C:28]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]2[C:26]1=[O:35].C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>CC(=O)CC>[CH:2]([NH:15][CH:16]1[CH2:21][CH2:20][N:19]([CH2:23][CH2:24][N:25]2[C:26](=[O:35])[C:27]3[C:28](=[CH:31][CH:32]=[CH:33][CH:34]=3)[C:29]2=[O:30])[CH2:18][CH2:17]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 113251H-Isoindole-1,3(2H)-dione, 2-(2-bromoethyl)-HCID 11430Potassium CarbonateHCID 70245335HCID 70245335、化合物

生成物 1

HCID 21187763HCID 21187763、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

The mixture of benzhydryl-piperidin-4-yl-amine hydrogen bromide salt (1.74 g, 5 mmol, 1.0 eq.), N-(2-bromoethyl)phthalimide (1.27 g, 5 mmol, 1.0 eq.), K2CO3 (1.73 g, 12.5 mmol, 2.5 eq.), and NaI (1.05 g, 7.0 mmol, 1.4 eq.) in 2-butanone (20 ml) was refluxed for 2-3 hours. The mixture was then cooled to room temperature. The white solid was filtered off and was washed with small amount of CHCl3. The filtrates were combined and concentrated. The resulted residue was dissolved in CHCl3 (100 ml). The solution was washed with water (3×20 ml), then dried over anhydrous Na2SO4. After removed all solvent, the crude product 2-{2-[4-(benzhydryl-amino)-piperidin-1-yl]-ethyl} -isoindole-1,3-dione was yielded (2.70 g).

後処理

  1. temperaturewas refluxed for 2-3 hours
  2. filtrationThe white solid was filtered off
  3. washwas washed with small amount of CHCl3
  4. concentrationconcentrated
  5. dissolutionThe resulted residue was dissolved in CHCl3 (100 ml)
  6. washThe solution was washed with water (3×20 ml)
  7. dry with materialdried over anhydrous Na2SO4
  8. customAfter removed all solvent

出典と根拠

ORDレコード
ord-024c91153859407cad07ff94336b5eeb
出典データセット
uspto-grants-2001_07
特許番号
US06255323B1

反応ノート

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