2-Methoxyethylamine → HCID 58459091, Verbindung

HRID 408808

Reaktionsgleichung

Reaktionsgleichung von HRID 408808
Cl[C:2]1[C:7]([NH2:8])=[C:6]([Cl:9])[N:5]=[C:4]([CH3:10])[N:3]=1.[CH3:11][O:12][CH2:13][CH2:14][NH2:15].C(N(C(C)C)CC)(C)C>C(O)(C)C.ClCCl>[Cl:9][C:6]1[N:5]=[C:4]([CH3:10])[N:3]=[C:2]([NH:15][CH2:14][CH2:13][O:12][CH3:11])[C:7]=1[NH2:8]

Komponenten

6

Edukt 3

HCID 80182-MethoxyethylamineHCID 81531DiisopropylethylamineHCID 7366744,6-Dichloro-2-methylpyrimidin-5-amine

Produkt 1

HCID 58459091HCID 58459091, VerbindungAusbeute 115,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Heat a solution of 4,6-dichloro-2-methyl-pyrimidin-5-ylamine (5.0 g, 0.02 mol), 2-methoxyethylamine (2.32 g, 0.03 mol) and diisopropylethylamine (3.9 g, 0.03 mol) in isopropanol (70 mL) at 150° C. in a sealed tube for 16 h. Cool the reaction mixture to room temperature, and remove the isopropanol under reduced pressure to give a residue. Dissolve the residue in dichloromethane and wash with water and brine. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Purify the residue on a silica gel column eluting with methanol:dichloromethane (4:96) to give the title compound (5.0 g). ES/MS m/z 217 (M+1).

Aufarbeitung

  1. customremove the isopropanol under reduced pressure
  2. customto give a residue
  3. washwash with water and brine
  4. dry with materialDry the organic layer over anhydrous sodium sulfate
  5. filtrationfilter
  6. concentrationconcentrate under reduced pressure
  7. customto give a residue
  8. customPurify the residue on a silica gel column
  9. washeluting with methanol:dichloromethane (4:96)

Quellen und Nachweise

ORD-Eintrag
ord-e1eff8e04c884e67bcddbb118d418b4e
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08759360B2

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