Water → HCID 18423142, Verbindung

HRID 1282137Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1282137
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=1.[C:14]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)(=[O:16])[CH3:15].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:14]([N:17]1[CH2:22][CH2:21][N:20]([CH2:2][C:3]2[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=2)[CH2:19][CH2:18]1)(=[O:16])[CH3:15]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 837951-AcetylpiperazineHCID 15550682N-((4-(chloromethyl)phenyl)methyl)acetamide

Produkt 1

HCID 18423142HCID 18423142, VerbindungAusbeute 102 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of N-(4-chloromethylphenylmethyl)acetamide (7.7 g), 1-acetylpiperazine (5.0 g) and potassium carbonate (8.1 g) in dimethylformamide (50 ml) was stirred at 80° C. for 5 hr. The reaction mixture was poured into water (250 ml) and extracted with chloroform. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a yellow oil. The obtained yellow oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1) to give the title compound (11.5 g) as a colorless transparent oil.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customto give a yellow oil
  6. customThe obtained yellow oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1)

Quellen und Nachweise

ORD-Eintrag
ord-90e0563654b4406fbcbe4cc01a6f02de
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06455528B1

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