Hydrazine → HCID 68514795, Verbindung

HRID 882749Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 882749
Cl[C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[N:5]=[C:4]([O:14][CH2:15][C:16]([CH3:19])([OH:18])[CH3:17])[CH:3]=1.[NH2:20][NH2:21]>O1CCOCC1>[NH:20]([C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[N:5]=[C:4]([O:14][CH2:15][C:16]([CH3:19])([OH:18])[CH3:17])[CH:3]=1)[NH2:21]

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 86243997HCID 86243997, Verbindung

Produkt 1

HCID 68514795HCID 68514795, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

1-(6-chloro-2-morpholin-4-yl-pyrimidin-4-yloxy)-2-methyl-propan-2-ol (2.58 g) was dissolved in dioxane (50 mL) and hydrazine (3 mL) was added. The solution was heated to reflux for one hour, at which point the solvent was evaporated. The solid was dissolved in dichloromethane (200 mL) and washed with 10% sodium carbonate (10 mL). The organic layer was dried over magnesium sulfate and evaporated to give 1-(6-hydrazino-2-morpholin-4-yl-pyrimidin-4-yloxy)-2-methyl-propan-2-ol, which was used without purification in the next reaction.

Aufarbeitung

  1. temperatureThe solution was heated
  2. temperatureto reflux for one hour, at which point the solvent
  3. customwas evaporated
  4. dissolutionThe solid was dissolved in dichloromethane (200 mL)
  5. washwashed with 10% sodium carbonate (10 mL)
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-1d44cfe3197d4ffeafd7d19d16987929
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08236795B2

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