反应详情

To 100 g (0.63 mol) of ethyl isobutyryl acetate was added ammonium acetate (68.2 g, 0.89 mol), cyclohexane (230 mL) and isopropanol (74 mL). The mixture was heated at reflux under argon atmosphere with a Dean-Stark trap. After 2 hours, a second portion of ammonium acetate (14.6 g, 0.19 mol) was added to the reaction. The reaction was heated at reflux for 12 hours and then allowed to cool to room temperature. A total of ˜30 mL of water was collected in the Dean-Stark trap. An ice bath was used to cool the reaction to 10° C. and then ammonium hydroxide (63 mL) was added dropwise. The organic layer was separated, dried with sodium sulfate, filtered, and concentrated to yield a yellow oil. The crude product (90.9 g, 0.58 mol, 92%) was taken directly to the next step without any further purification.

1. temperatureThe mixture was heated
2. temperatureat reflux under argon atmosphere with a Dean-Stark trap
3. temperatureThe reaction was heated
4. temperatureat reflux for 12 hours
5. customA total of ˜30 mL of water was collected in the Dean-Stark trap
6. customAn ice bath was used
7. temperatureto cool
8. customthe reaction to 10° C.
9. customThe organic layer was separated
10. dry with materialdried with sodium sulfate
11. filtrationfiltered
12. concentrationconcentrated
13. customto yield a yellow oil