反应详情

温度

80 °C

Concentrated H2SO4 (20 ml) is heated to 50° C. The compound obtained in Step D (25.24 mmoles) is added slowly in solid form, maintaining the temperature between 60 and 70° C. The reaction mixture is then stirred for one hour at 80° C. The mixture is brought to ambient temperature and then poured onto 200 g of crushed ice. After 30 minutes, the red solid formed is filtered off and washed intensively with ice-cold water; it is then dried in vacuo in the presence of P2O5 and at 40° C. overnight to yield the title product, which is used directly in the next Step.

1. temperaturemaintaining the temperature between 60 and 70° C
2. customis brought to ambient temperature
3. waitAfter 30 minutes
4. customthe red solid formed
5. filtrationis filtered off
6. washwashed intensively with ice-cold water
7. dry with materialit is then dried in vacuo in the presence of P2O5 and at 40° C. overnight