Triethylamine → 2-Methoxy-5-((4-methylpiperazin-1-yl)sulfonyl)benzoic acid

HRID 1012149

Reaktionsgleichung

Reaktionsgleichung von HRID 1012149
Cl[S:2]([C:5]1[CH:6]=[CH:7][C:8]([O:14][CH3:15])=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11])(=[O:4])=[O:3].[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(N(CC)CC)C>CC(C)=O>[CH3:15][O:14][C:8]1[CH:7]=[CH:6][C:5]([S:2]([N:20]2[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]2)(=[O:4])=[O:3])=[CH:13][C:9]=1[C:10]([OH:12])=[O:11]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 531671-MethylpiperazineHCID 1040075-Chlorosulphonyl-2-anisic acid

Produkt 1

HCID 112899822-Methoxy-5-((4-methylpiperazin-1-yl)sulfonyl)benzoic acidAusbeute 24 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To solution of 5-chlorosulphonyl-2-methoxy-benzoic acid (0.5 g, 1.99 mmol) in acetone (5 ml) was added N-methylpiperazine (0.219 g, 2.19 mmol) and triethylamine (0.33 ml, 2.3 mmol) and the mixture stirred at RT. After 2 hours the reaction mixture was filtered and the collected solid washed with acetone, water and then diethylether to yield 2-methoxy-5-(4-methyl-piperazine-1-sulphonyl)-benzoic acid (150 mg, 24%). (LC/MS (acidic method): Rt 0.34, [M+H]+ 315).

Aufarbeitung

  1. filtrationAfter 2 hours the reaction mixture was filtered
  2. washthe collected solid washed with acetone, water

Quellen und Nachweise

ORD-Eintrag
ord-8fa02af2661d432fb5da20e0397de61f
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977477B2

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