Cyclopropyl methyl ketone → 1-Cyclopropyl-3-(pyrimidin-4-yl)propane-1,3-dione

HRID 1076690

Reaktionsgleichung

Reaktionsgleichung von HRID 1076690
CO[C:3]([C:5]1[CH:10]=[CH:9][N:8]=[CH:7][N:6]=1)=[O:4].[CH:11]1([C:14]([CH3:16])=[O:15])[CH2:13][CH2:12]1.C[O-].[Na+]>C1C=CC=CC=1>[CH:11]1([C:14](=[O:15])[CH2:16][C:3]([C:5]2[CH:10]=[CH:9][N:8]=[CH:7][N:6]=2)=[O:4])[CH2:13][CH2:12]1

Komponenten

5

Edukt 3

HCID 13004Cyclopropyl methyl ketoneHCID 254248Methyl pyrimidine-4-carboxylateHCID 10942334Sodium Methoxide

Produkt 1

HCID 123605621-Cyclopropyl-3-(pyrimidin-4-yl)propane-1,3-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A stirred mixture of 1.4 g. of methyl-4-pyrimidinecarboxylate, 1.7 g. of cyclopropylmethyl ketone, 1.2 g. of sodium methoxide and 40 ml. of benzene is heated under reflux for 4 hours. The mixture is diluted with 40 ml. of water and the benzene phase is removed. The aqueous mixture is made weakly acidic with dilute hydrochloric acid and extracted with chloroform. The cloroform solution is dried over magnesium sulfate and concentrated under reduced pressure to give light brown crystals, which are recrystallized from hexane to provide straw-colored crystals, melting point 81°-84°C.

Aufarbeitung

  1. additionA stirred mixture of 1.4 g
  2. temperatureunder reflux for 4 hours
  3. additionThe mixture is diluted with 40 ml
  4. customof water and the benzene phase is removed
  5. extractionextracted with chloroform
  6. dry with materialThe cloroform solution is dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto give light brown crystals, which
  9. customare recrystallized from hexane
  10. customto provide straw-colored crystals, melting point 81°-84°C.

Quellen und Nachweise

ORD-Eintrag
ord-5a3ef876c5c24c87aba1951f6e7e9048
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03957805

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