4-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile monohydrochloride monohydrate → 4-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile

HRID 270631

Reaktionsgleichung

Reaktionsgleichung von HRID 270631
O.Cl.[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[CH2:11][C:12]1[N:17]=[C:16]([NH:18][OH:19])[N:15]=[C:14]([NH:20][C:21]2[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[CH:23][CH:22]=2)[N:13]=1>C(OC(=O)C)C>[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[CH2:11][C:12]1[N:17]=[C:16]([NH:18][OH:19])[N:15]=[C:14]([NH:20][C:21]2[CH:22]=[CH:23][C:24]([C:25]#[N:26])=[CH:27][CH:28]=2)[N:13]=1

Komponenten

3

Edukt 1

HCID 222816854-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile monohydrochloride monohydrate

Produkt 1

HCID 4864294-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrileAusbeute 70,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Compound (21) (0.00227 mol) was stirred in ethylacetate (50 ml). The mixture was washed with NaHCO3 (50 ml saturated solution), then washed with brine, dried, filtered and the solvent was evaporated. The residue was crystallized from methanol, filtered off and dried, yielding 0.60 g (70.6%) of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile (compound 33).

Aufarbeitung

  1. washThe mixture was washed with NaHCO3 (50 ml saturated solution)
  2. washwashed with brine
  3. customdried
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customThe residue was crystallized from methanol
  7. filtrationfiltered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f688cf125a5448d287e4e8b0016167c6
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07449575B2

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