Water → 10-butyl-mesityl-2,5-dimethyl-7,8,9,10-tetrahydro-6H-pyrazolo[5',1'-:2,3]pyrimido[4,5-b]azepine

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Reaktionsgleichung

[I].[Na].C(=O)([O-])[O-].[K+].[K+].C(N[C:14]1([CH2:34][CH2:35][CH2:36][CH2:37]Cl)[CH2:19][N:18]2[N:20]=[C:21]([CH3:32])[C:22]([C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])=[C:17]2[N:16]=[C:15]1[CH3:33])CCC.O>CN1CCCCC1=O>[CH2:15]([N:16]1[CH2:37][CH2:36][CH2:35][CH2:34][C:14]2[C:15]([CH3:33])=[N:16][C:17]3[N:18]([N:20]=[C:21]([CH3:32])[C:22]=3[C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])[C:19]1=2)[CH2:14][CH2:34][CH3:35]

Komponenten

Reaktionsbedingungen

Temperatur: 150 °C

Versuchsvorschrift

Sodium iodine (catalytic amount) and potassium carbonate (65 mg, 0.47 mmol) were added to a solution of N-butyl-N-(6-(4-chlorobutyl)-3-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-yl)amine (65 mg, 0.15 mmol) in 1-methyl-2-piperidone (2 mL), followed by stirring at 150° C. for four hours. Then, the mixture was treated with water, extracted with ethyl acetate, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel chromatography (15% ethyl acetate/hexane), to give the title compound (18 mg) as yellow crystals.

Aufarbeitung

extractionextracted with ethyl acetate
dry with materialdried over anhydrous magnesium sulfate
customevaporated
customThe residue was purified by silica gel chromatography (15% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag: ord-bef75e6bc70440dfb270579ffea4ba7d
Quelldatensatz: uspto-grants-2005_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06951865B2

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