Sodium Iodide → HCID 21187763, 화합물

HRID 1383458노트

반응식

HRID 1383458 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 21187763HCID 21187763, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-024c91153859407cad07ff94336b5eeb
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255323B1

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