反应详情

温度

30 °C

Mechanically stir mixture of 6-chloro-2-methyl-3-nitro-pyridine (Asymchem, 25.00 g, 144.9 mmol), tert-butyl 1-piperazinecarboxylate (29.68 g, 159.4 mmol), and triethylamine (23.2 mL, 167 mmol) in n-BuOH (250 mL) at 50° C. under nitrogen for 4 hours, at 65° C. for 2 hours, then at room temperature overnight. Add additional tert-butyl 1-piperazinecarboxylate (1.5 g), and heat the reaction at 65° C. for 4 hours. Cool the resulting slurry to 30° C. then add hexanes (75 mL). Cool the slurry to room temperature over 1 hour, then add water (150 mL). Allow the slurry to stand for 45 min then filter. Wash the cake with water (4×100 mL) then hexanes (100 mL) and air-dry overnight to yield 4-(6-methyl-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester as bright yellow crystals (46.30 g, 99% yield, MS(ES): m/z=267 [M+H—C4H8]).

1. customat room temperature
2. customovernight
3. temperatureheat
4. customthe reaction at 65° C. for 4 hours
5. temperatureCool the slurry to room temperature over 1 hour
6. waitto stand for 45 min
7. filtrationthen filter
8. washWash the cake with water (4×100 mL)
9. dry with materialhexanes (100 mL) and air-dry overnight