C 9 H 12 N 2 O 2 , triclinic, P¯ (no. 2), a = 6.6954(7) Å, b = 7.6325(8) Å, c = 9.8928(11) Å, α = 95.908(9)°, β = 92.810(9)°, γ = 108.360(8)°. V = 475.49(9) Å 3 , Z = 2, Rgt(F) = 0.0606, wR ref (F 2 ) = 0.1549, T = 296(2) K.
CCDC no.: 979896The gure shows the asymmetric unit of the title structure. Tables 1-3 contain details of the methods used and a
Source of materialA solution of ethyl 1,5-dimethyl-1H-pyrazole-3-carboxylate (12 mmol) in THF (25 mL) was added to a suspension of sodium (22 mmol) in THF (50 mL), and then acetone (1.2 g; 20.6 mmol) was added at 273 K. The resulting mixture was stirred at 273 K for 48 h and the formed residue was ltered, washed with THF, and neutralized with acetic acid to pH 5 after being dissolved in water. The organic layer was extracted with CH 2 Cl 2 , dried and concentrated in vacuum. The resulting mixture was chromatographed on silica using CH 2 Cl 2 as eluant to give the target product. Crystals suitable for Xray di raction analysis were obtained by slow evaporated of methanol from the mixture; yield: 37%; M.p. 356-357 K.