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Phosphorus oxychloride → 2-Chloro-5-isopropylpyrimidine

HRID 2251497
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2251497
[CH:1]([C:4]1[CH:5]=[N:6][C:7](=O)[NH:8][CH:9]=1)([CH3:3])[CH3:2].O=P(Cl)(Cl)[Cl:13]>CN(C)C1C=CC=CC=1>[Cl:13][C:7]1[N:6]=[CH:5][C:4]([CH:1]([CH3:3])[CH3:2])=[CH:9][N:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 123561535-Isopropylpyrimidin-2(1H)-one

Produkt 1

HCID 198466722-Chloro-5-isopropylpyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 949N,N-DimethylanilineKatalysator

Versuchsvorschrift

A mixture of 5-isopropylpyrimidin-2(1H)-one (2.1 g, 15.2 mmol), POCl3 (15 ml), and N,N-dimethylaniline (5 drops) was heated at reflux under a nitrogen atmosphere for 2 h. Upon cooling, the majority of the POCl3 was removed under reduced pressure. The residue was poured into ice water and extracted with chloroform (3×20 ml). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated to provide 2-chloro-5-isopropylpyrimidine as a light brown oil, which was used without further purification.

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Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux under a nitrogen atmosphere for 2 h
  3. temperatureUpon cooling
  4. customthe majority of the POCl3 was removed under reduced pressure
  5. additionThe residue was poured into ice water
  6. extractionextracted with chloroform (3×20 ml)
  7. washThe combined organic extracts were washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fb309df154684408a961ba21676f4e49
Quelldatensatz
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07319104B2

Notizen zur Reaktion

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