反应详情

1.00 g (3.68 millimole) of 15-hydroxy-12-ketopentadecanoic acid, 0.73 g (11.0 millimole) of 85 wt.% potassium hydroxide, 0.50 g (8.5 millimole) of 85 % hydrated hydrazine and 5 ml of diethylene glycol were charged into a frask and heated under reflux over 1.5 hours. Subsequently, while evaporating the produced light boiling components such as water to the outside of the system, the internal temperature was elevated to 195 to 205° C., and the heating under reflux was continued at the same temperature range over 2 hours. After completion of the reaction, the solution was cooled, diluted by addition of 5 ml of water and added with 3 ml of 6N-HCl, followed by collection of the precipitated pail brown solid by filtration. The solid was recrystallized from benzene to obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl.

1. temperatureheated
2. temperatureunder reflux over 1.5 hours
3. customSubsequently, while evaporating the produced light
4. customwas elevated to 195 to 205° C.
5. temperaturethe heating under reflux
6. customAfter completion of the reaction
7. temperaturethe solution was cooled
8. filtrationfollowed by collection of the precipitated pail brown solid by filtration
9. customThe solid was recrystallized from benzene
10. customto obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl