反应详情

温度

0 °C

To cyanoacetic acid (0.43 g, 5.12 mmol) in THF at −78° C., containing one crystal of 1,1′-bipyridyl was added n-butyl lithium (6.4 mL, 10.24 mmol). The temperature was allowed to warm to 0° C. resulting in a pink colored solution. After cooling to −78° C., 5-Methyl-3-phenyl-isoxazole-4-carbonyl chloride (0.567 g, 2.56 mmol) in THF (5 mL) was added dropwise. The mixture was stirred at −78° C. for 1 hr. and at ambient temperature for an addition 1 hr. The reaction was quenched with 1N HCl (13 mL0 and extracted twice with CH2Cl2. Combined extracts were washed with saturated NaHCO3, brine, dried over MgSO4 to give the title compound (0.391 g, 67% yield).

1. customresulting in a pink colored solution
2. temperatureAfter cooling to −78° C.
3. additionand at ambient temperature for an addition 1 hr
4. customThe reaction was quenched with 1N HCl (13 mL0
5. extractionextracted twice with CH2Cl2
6. washCombined extracts were washed with saturated NaHCO3, brine
7. dry with materialdried over MgSO4