Chlorotrimethylsilane → HCID 68509351, Verbindung
Reaktionsgleichung
[CH2:1]([C:3]1[NH:7][N:6]=[C:5]([C:8]([OH:10])=[O:9])[C:4]=1[CH3:11])[CH3:2].[Cl:12][Si](C)(C)[CH3:14]>CO>[ClH:12].[CH2:1]([C:3]1[NH:7][N:6]=[C:5]([C:8]([O:10][CH3:14])=[O:9])[C:4]=1[CH3:11])[CH3:2]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a mechanically stirred suspension of 5-ethyl-4-methyl-1H-pyrazole-3-carboxylic acid (1.0 g, 6.49 mmol) in dry methanol (30 mL) was added chlorotrimethylsilane (2.5 mL, 19.5 mmol). The reaction mixture was heated at reflux over night. After being cooled to rt, the solvent was removed in vacuo, and the residue was stirred in diethyl ether (20 mL) for 1 h. After filtration and vacuum drying the title compound was obtained as white crystals (832 mg, 63%): 1H NMR (400 MHz, CDCl3) δ 10.55 (broad, 1H), 4.00 (s, 3H), 2.91 (quart, 2H), 2.32 (s, 3H), 1.35 (t, 3H); ES-MS m/z 169 (MH)+; HPLC RT (Method F) 1.52 min.