Triethylamine → 4-Chloro-2-cyclopropyl-5-nitropyrimidine

HRID 2175200Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2175200
[CH:1]1([C:4]2[NH:9][C:8](=O)[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][N:5]=2)[CH2:3][CH2:2]1.C(N(CC)CC)C.P(Cl)(Cl)([Cl:23])=O>ClCCl>[Cl:23][C:8]1[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][N:5]=[C:4]([CH:1]2[CH2:3][CH2:2]2)[N:9]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 584974342-cyclopropyl-5-nitro-3H-pyrimidin-4-one

Produkt 1

HCID 567734194-Chloro-2-cyclopropyl-5-nitropyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a suspension of the 2-cyclopropyl-5-nitro-3H-pyrimidin-4-one (900 mg, 4.9 mmol) in dichloromethane (15 ml) was added triethylamine (505 mg, 5 mmol). To the clear solution obtained, phosphorous oxychloride (1.5 g, 10 mmol) was slowly added and the reaction mixture kept at room temperature for 2 hours. TLC showed a single spot. The reaction mixture was diluted with dichloromethane, washed with water and dried over MgSO4, filtered and evaporated to dryness to give brown oil. This material was used as such for the next step.

Aufarbeitung

  1. customTo the clear solution obtained
  2. washwashed with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customto give brown oil

Quellen und Nachweise

ORD-Eintrag
ord-834e20c56f5f441aa57c6800731ed1ed
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09062056B2

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