Propargyl bromide → HCID 12534513, Verbindung

HRID 1075178Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1075178
[K].[CH3:2][S:3][C:4]1[C:9]([F:10])=[CH:8][NH:7][C:6](=[O:11])[N:5]=1.[CH2:12](Br)[C:13]#[CH:14]>CN(C)C=O>[CH2:14]([N:7]1[CH:8]=[C:9]([F:10])[C:4]([S:3][CH3:2])=[N:5][C:6]1=[O:11])[C:13]#[CH:12]

Komponenten

5

Edukt 3

HCID 7842Propargyl bromideHCID 5462222PotassiumHCID 178503576HCID 178503576, Verbindung

Produkt 1

HCID 12534513HCID 12534513, VerbindungAusbeute 71 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The potassium salt of 4-methylthio-5-fluoropyrimid-2-one (0.005 mol) and propargyl bromide (0.06 mol) were stirred together in dimethylformamide (20 ml) for 40 hrs at room temperature. The mixture was then filtered; the filtrate evaporated at reduced pressure (1 mm Hg) and the residue extracted with chloroform (60 ml). The chloroform solution was washed with 1 N NaOH, with water, and dried (MgSO4) before evaporation; yield 71%, m.p. 101°-102° C. (ethyl acetate). (Found: C, 48.50; H, 3.62. Calc. for C8H7SN2O: C, 48.48; H, 3.56).

Aufarbeitung

  1. filtrationThe mixture was then filtered
  2. customthe filtrate evaporated at reduced pressure (1 mm Hg)
  3. extractionthe residue extracted with chloroform (60 ml)
  4. washThe chloroform solution was washed with 1 N NaOH, with water
  5. dry with materialdried (MgSO4)
  6. custombefore evaporation

Quellen und Nachweise

ORD-Eintrag
ord-022e3d27b56145c0855722b24b8f3648
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04395406

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