反应 #69390
ord-15f0e2379c1649a9a368f2866cef7f5d
反应方程式
thiosalicylic acid
sulfuric acid
phenol
→
2-hydroxy-thioxanthen-9-on
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他rose to 60° C
- 2workup.WAITto continue for 2 hours at 80° C
- 3workup.ADDITIONwas added slowly to 3 l
- 4workup.WAITThe mixture was kept at the boiling point for 5 minutes
- 5温度to cool down to room temperature
实验过程
16 g (103 mmol) thiosalicylic acid was slowly added to 150 mL concentrated sulfuric acid. The mixture is stirred for 5 minutes and 60 g (440 mmol) phenol was added over 30 minutes. The temperature rose to 60° C. The reaction was allowed to continue for 2 hours at 80° C. The reaction was allowed to cool down to room temperature and was added slowly to 3 l boiling water. The mixture was kept at the boiling point for 5 minutes. The mixture was allowed to cool down to room temperature. The precipitated 2-hydroxy-thioxanthen-9-on was isolated by filtration and dried. 14.1 g (63%) of 2-hydroxy-thioxanthen-9-on was isolated (m.p. 232-241° C.).