反应详情

温度

40 °C

Intermediate IV (150 g, 0.44 mol) was added to glacial acetic acid (8v/w, 1200 mL). The mixture was warmed up to 40° C. After Intermediate IV was dissolved completely, iron powder (123.1 g, 2.20 mol) was slowly added in batch. The mixture was warmed up to 80° C. and reacted under mechanical stirring for 2 h. After completion of the reaction, the reaction solution was filtered by suction when it is still hot. The filtrate was collected. After cooling the filtrate, a great deal of solid separated out and was filtered by suction to produce a lutescens solid. The filtered cake was dissolved in glacial acetic acid. The mixture was stirred at 80° C. for about 30 min, and was filtered by suction again when it is still hot. The filtrate was collected. After cooling the filtrate, a solid separated out and was filtered by suction to produce a lutescens solid. The solids were combined, and washed with water several times until the filtrate became neutral. The filtered cake was dried to produce a pale yellow solid (79 g) in a yield of 65%.

1. temperatureThe mixture was warmed up to 80° C.
2. customreacted
3. customAfter completion of the reaction
4. filtrationthe reaction solution was filtered by suction when it
5. customThe filtrate was collected
6. temperatureAfter cooling the filtrate
7. customa great deal of solid separated out
8. filtrationwas filtered by suction
9. customto produce a lutescens solid
10. stirringThe mixture was stirred at 80° C. for about 30 min
11. filtrationwas filtered by suction again when it
12. customThe filtrate was collected
13. temperatureAfter cooling the filtrate
14. customa solid separated out
15. filtrationwas filtered by suction
16. customto produce a lutescens solid
17. washwashed with water several times until the filtrate
18. customThe filtered cake was dried