反应详情

温度

52.5 °C

Neat anhydrous hydrazine 21.0 g (654 mmol) was added to a solution of p-hydroxyphenylacetic acid methyl ester 27.18 g (163.5 mmol) in MeOH (100 mL) and the mixture was heated to 50-55° C. and stirred at this temperature for 90 min (water bath). Cooled, stirred for extra 1 hour, the precipitate collected by filtration, compressed on the frit, washed with MeOH (3×10 mL) and dried on high vacuum. A second fraction was obtained by cooling the supernatants to −15° C. overnight and filtering the formed precipitate.

1. temperatureCooled
2. filtrationthe precipitate collected by filtration
3. washwashed with MeOH (3×10 mL)
4. customdried on high vacuum
5. customA second fraction was obtained
6. temperatureby cooling the supernatants to −15° C. overnight
7. filtrationfiltering the formed precipitate