反应详情

温度

80 °C

NaH (0.234 g, 5.84 mmol) in dry toluene (5 ml) was heated to 80° C. A mixture of acetonitrile (0.229 ml, 4.38 mmol), ethyl 1-piperidineacetate (0.5 g, 2.92 mmol) and toluene (3 ml) was added dropwise to the hot reaction mixture. The mixture was stirred at 80° C. for 1.5 hours and after cooling to RT, quenched by the addition of water (6 ml). Hydrazine hydrate (0.142 ml, 2.92 mmol) was added and reaction mixture reheated to 80° C. for 3 hours. The reaction mixture was acidified with 2N HCl (aq.) to pH 2 and loaded onto a SCX-2 cartridge eluting with MeOH followed by 7M NH3 in MeOH. The methanolic ammonia fractions were concentrated in vacuo to afford an oil. 4N HCl in dioxane (15 ml) was added to the yellow oil and the resulting suspension was filtered and washed with iso-hexane to yield the title compound.

1. additionwas added dropwise to the hot reaction mixture
2. temperatureafter cooling to RT
3. customquenched by the addition of water (6 ml)
4. customreaction mixture
5. waitreheated to 80° C. for 3 hours
6. washeluting with MeOH
7. concentrationThe methanolic ammonia fractions were concentrated in vacuo
8. customto afford an oil
9. filtrationthe resulting suspension was filtered
10. washwashed with iso-hexane