Iodoethane → 6-ethyl-7,8-dihydroimidazo[1,5-c]pyrimidin-5(6H)-one

HRID 333415Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 333415
[O:1]=[C:2]1[N:7]2[CH:8]=[N:9][CH:10]=[C:6]2[CH2:5][CH2:4][NH:3]1.[H-].[Na+].I[CH2:14][CH3:15]>CN(C=O)C>[CH2:14]([N:3]1[CH2:4][CH2:5][C:6]2=[CH:10][N:9]=[CH:8][N:7]2[C:2]1=[O:1])[CH3:15]

Komponenten

5

Edukt 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 14875185H,6H,7H,8H-imidazo(1,5-c)pyrimidin-5-one

Produkt 1

HCID 126472846-ethyl-7,8-dihydroimidazo[1,5-c]pyrimidin-5(6H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To 500 mg (3.6 mmol) of 5,6,7,8-tetrahydro-5-oxoimidazo[1,5-c]pyrimidine dissolved in 5 mL of DMF are added cautiously at room temperature 173 mg (4.32 mmol) of sodium hydride. The reaction medium is stirred for 1 hour at room temperature, and 0.35 mL (4.32 mmol) of iodoethane is then added dropwise. The reaction medium is stirred for 2 hours at room temperature and the solvents are then evaporated off. The residue is treated with 1N NaHCO3 solution and extracted with chloroform. The combined organic phases are dried with MgSO4, filtered and evaporated. The oil obtained is used directly in the following step.

Aufarbeitung

  1. stirringThe reaction medium is stirred for 2 hours at room temperature
  2. customthe solvents are then evaporated off
  3. additionThe residue is treated with 1N NaHCO3 solution
  4. extractionextracted with chloroform
  5. dry with materialThe combined organic phases are dried with MgSO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe oil obtained

Quellen und Nachweise

ORD-Eintrag
ord-b9fc3996d22b4207a971a1dc312ba64b
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08877968B2

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