Triethylamine → HCID 23206746, Verbindung

HRID 399737

Reaktionsgleichung

Reaktionsgleichung von HRID 399737
[CH3:1][C:2]([CH3:29])([P:26](=[O:28])=[O:27])[N:3]([C:15]1[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([O:22][CH2:23][CH2:24][NH2:25])[CH:16]=1)[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13][CH3:14])(=[O:6])=[O:5].[Cl:30][C:31]1[N:32]=[N:33][CH:34]=[C:35](Cl)[C:36]=1[Cl:37].C(N(CC)CC)C>O1CCCC1>[CH3:1][C:2]([CH3:29])([P:26](=[O:28])=[O:27])[N:3]([C:15]1[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([O:22][CH2:23][CH2:24][NH:25][C:35]2[C:36]([Cl:37])=[C:31]([Cl:30])[N:32]=[N:33][CH:34]=2)[CH:16]=1)[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13][CH3:14])(=[O:5])=[O:6]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 701113,4,5-TrichloropyridazineHCID 23206743HCID 23206743, Verbindung

Produkt 1

HCID 23206746HCID 23206746, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

940 mg N-(dimethyloxophosphinyl-methyl)-N-[3-(2-amino-ethoxy)-5-methyl-phenyl]-2-methoxy-benzene sulfonamide, 400 mg (2.2 mmol) 3,4,5-trichloropyridazine and 0.31 ml (2.2 mmol) triethylamine in 20 ml dry tetrahydrofuran were stirred for 2 h at 80° C., the solvent was removed in a vacuum, the residue was stirred with water, extracted three times with ethyl acetate, dried over sodium sulfate, filtered, the solvent was removed in a vacuum and 1.26 g (quant.) of a mixture of N-(dimethyloxophosphinyl-methyl)-N-{3-[2-(3,5-dichloropyridazin-4-ylamino)-ethoxy]-5-methylphenyl-}-2-methoxy-benzenesulfonamide and N-(dimethyloxophosphinyl-methyl)-N-{3-[2-(3,4-dichloropyridazin-5-ylamino)-ethoxy]-5-methylphenyl}-2-methoxy-benzenesulfonamide was obtained as an oil. MS (m/e)=573.

Aufarbeitung

  1. customthe solvent was removed in a vacuum
  2. extractionextracted three times with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent was removed in a vacuum and 1.26 g (quant.) of a mixture of N-(dimethyloxophosphinyl-methyl)-N-{3-[2-(3,5-dichloropyridazin-4-ylamino)-ethoxy]-5-methylphenyl-}-2-methoxy-benzenesulfonamide

Quellen und Nachweise

ORD-Eintrag
ord-0acf224e00e245e3b74cc0b9a8d9a17c
Quelldatensatz
uspto-grants-1998_10
Patentnummer
US05824679

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