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Stage #1: With sodium hydride In N,N-dimethyl-formamide; mineral oil at 0℃; for 1 h; Inert atmosphere Stage #2: at 20℃;
1003101 Step A: Preparation of methyl 1-methyl-1H-1,2,4-triazole-3-carboxylate: To a stirred suspension of Nail (60percent oil dispersion, 0.346 g, 8.66 mmol) in DMF (20 mL) was added dropwise a solution of methyl 1H-1,2,4-triazole-3-carboxylate (1.00 g, 7.87 mmol) in DMF (20 mE) at 0 °C under nitrogen. The reaction mixture was stirred at 0 °C for 1 hour. Mel (0.982 mL, 15.7 mmol) was added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction was poured into cold water and extracted with EtOAc. The combined organic layers were washed with brine, dried and concentrated. The residue was purified by column chromatography (3:1 hexanes/EtOAc) to give the title compound (0.380 g, 34percent yield) as a white solid. MS (apci) mlz = 142.1 (M+H).
34%
Stage #1: With sodium hydride In N,N-dimethyl-formamide; mineral oil at 0℃; for 1 h; Inert atmosphere Stage #2: at 20℃;
[00430] Step A: Preparation of methyl l-methyl-lH-L2,4-triazole-3-carboxylate: To a stirred suspension of NaH (60percent oil dispersion, 0.346 g, 8.66 mmol) in DMF (20 mL) was added dropwise a solution of methyl lH-l,2,4-triazole-3-carboxylate (1.00 g, 7.87 mmol) in DMF (20 mL) at 0 °C under nitrogen. The reaction mixture was stirred at 0 °C for 1 hour. Mel (0.982 mL, 15.7 mmol) was added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction was poured into cold water and extracted with EtOAc. The combined organic layers were washed with brine, dried and concentrated. The residue was purified by column chromatography (3: 1 hexanes/EtOAc) to give the title compound (0.380 g, 34percent yield) as a white solid. MS (apci) m/z = 142.1 (M+H).
34%
Stage #1: With sodium hydride In N,N-dimethyl-formamide; mineral oil at 0℃; for 1 h; Inert atmosphere Stage #2: at 20℃;
[00614] Step A: Preparation of methyl 1-methyl-1H-1,2,4-triazole-3-carboxylate: To a stirred suspension of NaH (60percent oil dispersion, 0.346 g, 8.66 mmol) in DMF (20 mL) was added dropwise a solution of methyl 1H-1,2,4-triazole-3-carboxylate (1.00 g, 7.87 mmol) in DMF (20 mE) at 0 °C under nitrogen. The reaction mixture was stirred at 0 °C for 1 hour. Mel (0.982 mL, 15.7 mmol) was added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction was poured into cold water and extracted with EtOAc. The combined organic layers were washed with brine, dried and concentrated. The residue was purified by column chromatography (3:1 hexanes/EtOAc) to give the title compound (0.380 g, 34percent yield) as a white solid. MS (apci) m/z = 142.1 (M+H).
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