反应详情

温度

35 °C

A mixture of 50 g of the compound of Example 2, 34 g of sodium formate and 505 ml of formic acid was warmed to 35° C. and 90 ml of 30% hydrogen peroxide was added slowly over 0.75 hours. The reaction temperature was allowed to warm to 55° C. and held at 55° C. for 2 hours. The reaction mixture was cooled to ambient temperature and 7 g of sodium sulfite was added in portions to destroy excess hydrogen peroxide. The reaction mixture was concentrated in vacuo at 50° C. Toluene (250 ml) was added to the residue, and the suspension was concentrated in vacuo. Repeating this procedure gave 109 g of the title compound as a moist white solid, m.p. >280° C.

1. temperatureto warm to 55° C.
2. temperatureThe reaction mixture was cooled to ambient temperature
3. customto destroy excess hydrogen peroxide
4. concentrationThe reaction mixture was concentrated in vacuo at 50° C
5. additionToluene (250 ml) was added to the residue
6. concentrationthe suspension was concentrated in vacuo