反应详情

温度

110 °C

7.7 g (40 mmole) of 2-methyl-4-oxo-4-phenylbutanoic acid was added to a 100 ml single-necked round bottom flask followed by 3.0 ml (60 mmole) of hydrazine monohydrate and then 20 ml of reagent grade ethanol (100%, 95% of ethanol should be fine also). The flask was fitted with a reflux condenser and the reaction mixture was heated to reflux in an oil bath at 110° C. (temperature of oil bath) and stirred for 2 h. The flask was then removed from the oil bath and the reaction mixture cooled to ambient temperature. The stir bar was removed and the solvent was evaporated in vacuo in a water bath at 45° C. The residue was then treated with 50 ml of Milli-Q water and stirred for 10 minutes to give a suspension. The precipitate was collected by filtering, washed with 100 ml of 2N NaHCO3, then washed with 60 ml Milli-Q water three times, and dried over a medium frit sintered glass funnel in vacuo to give 7.15 g of white crystals (Syn. ID, WH-8-004). Yield, 95%, confirmed by ESI-MS. ESI-MS: m/z 189.2 (M+H+).

1. customThe flask was fitted with a reflux condenser
2. temperaturethe reaction mixture was heated
3. customThe flask was then removed from the oil bath
4. temperaturethe reaction mixture cooled to ambient temperature
5. customThe stir bar was removed
6. customthe solvent was evaporated in vacuo in a water bath at 45° C
7. additionThe residue was then treated with 50 ml of Milli-Q water
8. stirringstirred for 10 minutes
9. customto give a suspension
10. customThe precipitate was collected
11. filtrationby filtering
12. washwashed with 100 ml of 2N NaHCO3
13. washwashed with 60 ml Milli-Q water three times
14. customdried over a medium frit sintered glass funnel in vacuo