Hydroxyamine hydrochloride → HCID 25009625, Verbindung

HRID 14992Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 14992
[CH3:1][N:2]1[C:15]2[CH:14]=[C:13]([CH:16]([CH2:26][CH:27]3[CH2:32][CH2:31][C:30](=O)[CH2:29][CH2:28]3)[C:17]([NH:19][C:20]3[CH:24]=[CH:23][N:22]([CH3:25])[N:21]=3)=[O:18])[CH:12]=[CH:11][C:10]=2[S:9](=[O:35])(=[O:34])[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.Cl.[NH2:37][OH:38]>CO>[OH:38][N:37]=[C:30]1[CH2:31][CH2:32][CH:27]([CH2:26][CH:16]([C:13]2[CH:12]=[CH:11][C:10]3[S:9](=[O:34])(=[O:35])[C:8]4[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=4)[N:2]([CH3:1])[C:15]=3[CH:14]=2)[C:17]([NH:19][C:20]2[CH:24]=[CH:23][N:22]([CH3:25])[N:21]=2)=[O:18])[CH2:28][CH2:29]1

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 24864113HCID 24864113, Verbindung

Produkt 1

HCID 25009625HCID 25009625, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

67 mg of 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-N-(1-methyl-1H-pyrazol-3-yl)-3-(4-oxocyclohexyl)propionamide and 14 mg of hydroxylamine hydrochloride are dissolved in 13 ml of methanol and heated at the boil under reflux for three hours. The methanol is then removed under reduced pressure, and the resulting residue is taken up in a mixture of 20 ml of ethyl acetate and 10 ml of water. The organic phase is washed twice with in each case 10 ml of water, dried over MgSO4, concentrated under reduced pressure and then lyophilized. This gives 49 mg of 3-(4-hydroxyiminocyclohexyl)-2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-N-(1-methyl-1H-pyrazol-3-yl)propionamide.

Aufarbeitung

  1. temperatureheated at the boil
  2. temperatureunder reflux for three hours
  3. customThe methanol is then removed under reduced pressure
  4. additionthe resulting residue is taken up in a mixture of 20 ml of ethyl acetate and 10 ml of water
  5. washThe organic phase is washed twice with in each case 10 ml of water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1cb44697a2c046d5a471bac03c1dbbb1
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07732440B2

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