反应详情

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. temperatureto reflux in an oil bath at 110 C (temperature of oil bath)
4. customThe flask was then removed from the oil bath
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