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Piperazine → 4-[2-(3,5-Dichloro-4-pyridyl)-1-oxoethyl]-2-(1-piperazinyl)carbonyl-7-methoxybenzofuran

HRID 1937425
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1937425
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:25])[C:7]=1[CH2:8][C:9]([C:11]1[C:16]2[CH:17]=[C:18]([C:20]([OH:22])=O)[O:19][C:15]=2[C:14]([O:23][CH3:24])=[CH:13][CH:12]=1)=[O:10].O.ON1C2C=CC=CC=2N=N1.[NH:37]1[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]1>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:25])[C:7]=1[CH2:8][C:9]([C:11]1[C:16]2[CH:17]=[C:18]([C:20]([N:37]3[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]3)=[O:22])[O:19][C:15]=2[C:14]([O:23][CH3:24])=[CH:13][CH:12]=1)=[O:10]
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Komponenten

5

Edukt 3

HCID 4837PiperazineHCID 27960291-Hydroxybenzotriazole hydrateHCID 227341684-[2-(3,5-Dichloro-4-pyridyl)-1-oxoethyl]-7-methoxybenzofuran-2-carboxylic acid

Produkt 1

HCID 98682784-[2-(3,5-Dichloro-4-pyridyl)-1-oxoethyl]-2-(1-piperazinyl)carbonyl-7-methoxybenzofuranAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel
2×

Versuchsvorschrift

Compound M (4.12 g) obtained in Reference Example 3 was dissolved in DMF (150 ml), 1-hydroxybenzotriazole monohydrate (5.8 g) and N-ethyl-N-′3-dimethylaminopropylcarbodiimide monohydrochloride (8.2 g) were added thereto, and the mixture was stirred at room temperature for 10 minutes. The mixture was dropwise added to a solution of piperazine (18.6 g) in DMF (300 ml) and the mixture was stirred at room temperature for 12 hours. The solvent was distilled off under reduced pressure and the residue was extracted with chloroform. The extract was washed a saturated aqueous sodium chloride solution and dried over sodium sulfate, and the solvent was distilled off. The resulting residue was suspended in ethanol and the precipitated crystals were collected by filtration to give the desired compound (3.54 g, 73%) as colorless crystals.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. extractionthe residue was extracted with chloroform
  4. washThe extract was washed a saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. distillationthe solvent was distilled off
  7. filtrationthe precipitated crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-dd6b5fb6846f46748d51f69951c524a0
Quelldatensatz
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06395738B1

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