Chlorosuccinimide → 3,7-Dichloro-5-ethylpyrazolo[1,5-a]pyrimidine

HRID 1450371Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1450371
[Cl:1][C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([CH2:11][CH3:12])[CH:3]=1.[Cl:13]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Cl:13][C:10]1[CH:9]=[N:8][N:7]2[C:2]([Cl:1])=[CH:3][C:4]([CH2:11][CH3:12])=[N:5][C:6]=12

Komponenten

4

Edukt 2

HCID 31398ChlorosuccinimideHCID 105354107-Chloro-5-ethylpyrazolo[1,5-a]pyrimidine

Produkt 1

HCID 106324843,7-Dichloro-5-ethylpyrazolo[1,5-a]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

5.5 g (30 mmol) of the chloro compound (Example 1, Step B) and 4.0 g (30 mmol) of N-chlorosuccinimide were dissolved in 150 ml chloroform, stirred for 4 h at room temperature, and finally heated for some minutes on a steam bath. The mixture was poured on to ice water, the aqueous layer extracted with dichloromethane, the combined organic layers washed twice with saturated sodium carbonate solution, dried over sodium sulfate, and evaporated in in vacuo. The title compound was obtained as an oil after chromatography on silica gel with dichloromethane.

Aufarbeitung

  1. temperaturefinally heated for some minutes on a steam bath
  2. extractionthe aqueous layer extracted with dichloromethane
  3. washthe combined organic layers washed twice with saturated sodium carbonate solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated in in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7bb056b913c64aea94f5a54215db64f2
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05602137

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