反应详情

温度

50 °C

A mixture of 6-chloro-2-oxo-4-phenyl-1,2-dihydro-quinoline-3-carboxylic acid methyl ester (380 mg, 1.21 mmol, Eq: 1.00) and lithium hydroxide (3.8 ml, 3.8 mmol, Eq: 3.14) in ethanol (7.6 ml) was heated to 50° C. for 72 h in a sealed tube. Then water was added and the mixture was extracted with diethylether (3×). The pH of the aqueous layer was then adjusted to 1 by addition of 1N HCl and the mixture was extracted with ethyl acetate (3×). The combined ethyl acetate extracts were washed with brine, dried with Na2SO4 and evaporated to yield the title compound (378 mg) as off-white solid. MS (ESI): 300.0 (M+H)+.

1. extractionthe mixture was extracted with diethylether (3×)
2. additionThe pH of the aqueous layer was then adjusted to 1 by addition of 1N HCl
3. extractionthe mixture was extracted with ethyl acetate (3×)
4. washThe combined ethyl acetate extracts were washed with brine
5. dry with materialdried with Na2SO4
6. customevaporated