HCID 18374925, Verbindung → HCID 9877992, Verbindung

HRID 2300064Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2300064
[CH3:1][N:2]1[C:7]2[N:8]=[C:9](S(C)(=O)=O)[N:10]=[CH:11][C:6]=2[CH:5]=[CH:4][C:3]1=[O:16]>C(N)CCC>[CH2:3]([NH:2][C:9]1[N:10]=[CH:11][C:6]2[CH:5]=[CH:4][C:3](=[O:16])[N:2]([CH3:1])[C:7]=2[N:8]=1)[CH2:4][CH2:5][CH3:6]

Komponenten

3

Edukt 1

HCID 18374925HCID 18374925, Verbindung

Produkt 1

HCID 9877992HCID 9877992, VerbindungAusbeute 159,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8007ButylamineLösungsmittel

Versuchsvorschrift

A solution of 8-methyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one (200 mg, 0.83 mmol) in 2 mL of n-butylamine was stirred at room temperature for 10 minutes. The reaction mixture was partitioned between ethyl acetate and water, and the organic layer was washed with saturated sodium bicarbonate and brine, dried over magnesium sulfate, and concentrated in vacuo. A 4:1 mixture of hexane:ethyl acetate was added to the residue and the resultant solid collected by filtration to give 154 mg (79%) of 2-butylamino-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one, mp 146-147° C.

Aufarbeitung

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. washthe organic layer was washed with saturated sodium bicarbonate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. additionA 4:1 mixture of hexane
  6. additionethyl acetate was added to the residue
  7. filtrationthe resultant solid collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-1af32eed8c99406daa91afaab1806f40
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06498163B1

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