反应详情

温度

60 °C

To a solution of 2-chloro-3-methyl-5-nitropyridine (35 g, 200 mmol) in EtOH (400 mL) was added hydrazine hydrate (30.0 g, 600 mmol) and the resulting reaction mixture was stirred at 60° C. for 1 hr. The reaction mixture was cooled down with an ice bath, the resulting precipitate was filtrated off, washed with cold H2O and Et2O and dried at 50° C. under reduced pressure to afford the title product (25.40 g, 113 mmol, 98%) as a yellow solid. tR: 0.43 min (LC-MS 2); ESI-MS: 169 [M+H]+; ESI-MS: 167 [M−H]− (LC-MS 2).

1. customthe resulting reaction mixture
2. temperatureThe reaction mixture was cooled down with an ice bath
3. filtrationthe resulting precipitate was filtrated off
4. washwashed with cold H2O and Et2O
5. customdried at 50° C. under reduced pressure