Dimethylamine → HCID 178483319, Verbindung

HRID 241021Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 241021
Cl[CH2:2][C:3]1[N:12]=[C:11]([OH:13])[C:10]2[CH2:9][C:8]([CH3:15])([CH3:14])[CH2:7][CH2:6][C:5]=2[N:4]=1.[CH3:16][NH:17][CH3:18]>C1COCC1>[CH3:16][N:17]([CH2:2][C:3]1[N:12]=[C:11]([OH:13])[C:10]2[CH2:9][C:8]([CH3:15])([CH3:14])[CH2:7][CH2:6][C:5]=2[N:4]=1)[CH3:18]

Komponenten

4

Edukt 2

HCID 674DimethylamineHCID 1784239482-(chloromethyl)-6,6-dimethyl-1,5,7,8-tetrahydroquinazolin-4-one

Produkt 1

HCID 178483319HCID 178483319, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 2-(chloromethyl)-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol (2.5 g, 11 mmol) in THF (10 mL) was added dimethyl amine (2M in THF, 16.5 mL, 33 mmol). The reaction mixture was heated (60° C.) for two hours and then partitioned between ethyl acetate and sodium bicarbonate. The organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated to provide 2-((dimethylamino)methyl)-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol, which was used in step 3 without further purification. MS (ES) for C13H21N3O: 236 (MH+).

Aufarbeitung

  1. custompartitioned between ethyl acetate and sodium bicarbonate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-317c0e981c1b485f9551ee3e36ea7919
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08648066B2

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