Morpholine → HCID 58552871, Verbindung

HRID 520500Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 520500
Cl[CH2:2][C:3]1[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][N:4]=1.[NH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.C(N(CC)CC)C>C(O)C>[O:13]1[CH2:14][CH2:15][N:10]([CH2:2][C:3]2[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][N:4]=2)[CH2:11][CH2:12]1

Komponenten

5

Edukt 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 212988272-(Chloromethyl)pyrimidin-4-amine

Produkt 1

HCID 58552871HCID 58552871, VerbindungAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-(chloromethyl)pyrimidin-4-amine 126 (30.0 g, 209 mmol), morpholine 63 (23.7 g, 272 mmol) and triethylamine (42.3 g, 418 mmol) in anhydrous ethanol (250 mL) was heated at reflux for 16 h. The solvent was removed in vacuo and methanol (400 mL), H2O (100 mL) and sodium bicarbonate (25.0 g) were added. Stirring was continued for 30 min. The mixture was concentrated and purified by flash chromatography (dichloromethane: methanol: triethylamine=100:8:0.5) to give 127 (25.0 g, 62% yield).

Aufarbeitung

  1. temperatureat reflux for 16 h
  2. customThe solvent was removed in vacuo and methanol (400 mL), H2O (100 mL) and sodium bicarbonate (25.0 g)
  3. additionwere added
  4. concentrationThe mixture was concentrated
  5. custompurified by flash chromatography (dichloromethane: methanol: triethylamine=100:8:0.5)

Quellen und Nachweise

ORD-Eintrag
ord-300ac38009f24990ad7e84d6fd425a73
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09326986B2

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