Dimethylformamide → HCID 13338435, Verbindung

HRID 2417688Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2417688
Cl[C:2]1[C:3]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:4]=2[N:5]=[C:6]([CH3:8])[N:7]=1.[NH2:14][CH:15]([CH3:19])[C:16](=[O:18])[CH3:17].C(N([CH2:25][CH3:26])CC)C.CN(C)C=[O:30]>>[CH3:12][N:11]1[C:3]2[C:2]([NH:14][CH:15]([C:16]3([CH3:17])[O:30][CH2:25][CH2:26][O:18]3)[CH3:19])=[N:7][C:6]([CH3:8])=[N:5][C:4]=2[C:9]([CH3:13])=[N:10]1

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 44721173-Amino-2-butanoneHCID 133384077-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine

Produkt 1

HCID 13338435HCID 13338435, VerbindungAusbeute 87 %

Versuchsvorschrift

A mixture of 9.5 g (0.05 mol) of 7-chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine (Example 3), 10 g (0.075 mol) of 3-amino-2-butanone, ethylene ketal, and 14 ml of triethylamine in 30 ml of dimethylformamide is stirred at 50°-55° C. for 24 hours. The mixture is evaporated in vacuo, the residue is dissolved in methylene dichloride and washed with ammonium hydroxide solution. The organic layer is dried over MgSO4 and evaporated in vacuo. The residue is crystallized from pet ether to give 12.6 g (87%) of 1,3,5-trimethyl-N-[1-(2-methyl-1,3-dioxolan-2-yl)ethyl]-1H-pyrazol[4,3-d]pyrimidin-7-amine, mp 101°-103° C.

Aufarbeitung

  1. customThe mixture is evaporated in vacuo
  2. dissolutionthe residue is dissolved in methylene dichloride
  3. washwashed with ammonium hydroxide solution
  4. dry with materialThe organic layer is dried over MgSO4
  5. customevaporated in vacuo
  6. customThe residue is crystallized from pet ether

Quellen und Nachweise

ORD-Eintrag
ord-9fa8df680800474a888a1a2228cdd425
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04469868

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