反应详情

温度

10 °C

To a solution of cyclooctylamine (12.7 g., 0.10 mole) in chloroform (50 ml.) at 10°-20° C. is added dropwise ethyloxalyl chloride (6.83 g., 0.05 mole) in chloroform (50 ml.) over a period of 30 minutes. After stirring for 2 additional hours at 10° C., the mixture is washed with H2O (4×50 ml.), and the organic layer dried over Na2SO4. After filtration and evaporation an oil is obtained (11.3 g.). To the crude ethyl N-cyclooctyloxamate dissolved in ethanol (27 ml.) is added sodium (1.15 g., 0.05 mole) dissolved in absolute ethanol (35 ml.) and the mixture is stirred overnight. Following evaporation, the residue is dissolved in H2O (41 ml.) with heating, and the solution filtered while hot. The filtrate is acidified with 6 N HCl, and the resulting slurry cooled at ice temperature. The solid obtained by filtration is recrystallized from boiling H2O (100 ml.) to give N-cyclooctyloxamic acid, m.p. 115°-116° C.

1. washthe mixture is washed with H2O (4×50 ml.)
2. dry with materialthe organic layer dried over Na2SO4
3. filtrationAfter filtration and evaporation an oil
4. customis obtained (11.3 g.)
5. stirringthe mixture is stirred overnight
6. customevaporation
7. dissolutionthe residue is dissolved in H2O (41 ml.)
8. temperaturewith heating
9. filtrationthe solution filtered while hot
10. temperaturethe resulting slurry cooled at ice temperature
11. customThe solid obtained by filtration
12. customis recrystallized