Ethyl Acetate → HCID 59636159, Verbindung

HRID 80032Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 80032
Cl[CH2:2][CH2:3][CH2:4][NH:5][C:6]([NH:8][C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)=[O:7].[H-].[Na+].C(OCC)(=O)C>CN(C=O)C.C1COCC1>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([N:8]2[CH2:2][CH2:3][CH2:4][NH:5][C:6]2=[O:7])[CH:10]=1

Komponenten

6

Edukt 3

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 596362321-(3-Chloropropyl)-3-pyridin-3-ylurea

Produkt 1

HCID 59636159HCID 59636159, VerbindungAusbeute 97,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1-(3-Chloro-propyl)-3-pyridin-3-yl-urea (I-10a: 2.1 g, 9.859 mmol) in dry DMF (10 mL) was added to a solution of sodium hydride (487 mg, 10.154 mmol) in THF (2 mL) at 0° C. The reaction temperature was maintained at room temperature for 30 minutes. The reaction was monitored by TLC (100% ethyl acetate). The reaction mixture was quenched with MeOH (5 mL) at 0° C., concentrated under reduced pressure and partitioned between ice cold water and chloroform. The organic layer was dried over Na2SO4, and concentrated under reduced pressure to afford 1.7 g (97.14% yield) of 1-pyridin-3-yl-tetrahydro-pyrimidin-2-one.

Aufarbeitung

  1. customThe reaction mixture was quenched with MeOH (5 mL) at 0° C.
  2. concentrationconcentrated under reduced pressure
  3. custompartitioned between ice cold water and chloroform
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1dcb5e71067742dfb6d66a417d9f7fe1
Quelldatensatz
uspto-grants-2014_09
Patentnummer
USRE045173E1

Notizen zur Reaktion

Wird geladen…