反应 #71013

ord-8b29f5dd6897410091109be9c60f3e7e

反应方程式

O=C(O)c1ccccc1S
thiosalicylic acid
O=S(=O)(O)O
sulfuric acid
Oc1ccccc1
phenol
O=c1c2ccccc2sc2ccc(O)cc12
2-hydroxy-thioxanthen-9-on

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他rose to 60° C
  2. 2
    workup.WAITto continue for 2 hours at 80° C
  3. 3
    workup.WAITThe mixture was kept at the boiling point for 5 minutes
  4. 4
    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 31 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.)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08536217B2uspto-grants-2013_09