反应 #2460300

ord-e4077168dc75468aa1950b9c830a5b79

反应方程式

O=C(O)c1ccc(I)cc1
4-iodobenzoic acid
O=C(O)c1ccccc1S
thiosalicylic acid
O=C(O)c1ccc(Sc2ccccc2C(=O)O)cc1
2,4′-thiobis(benzoic acid)

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 5 h
  3. 3
    温度cooled
  4. 4
    过滤The reaction mixture was filtered
  5. 5
    其他The precipitate was collected
  6. 6
    洗涤washed with water
  7. 7
    workup.DISSOLUTIONdissolved
  8. 8
    过滤filtered
  9. 9
    浓缩The filtrate was concentrated

实验过程

First, 2,4′-thiobis(benzoic acid) was prepared. A mixture of 4-iodobenzoic acid (55.7 g, 225 mmol), thiosalicylic acid (34.6 g, 225 mmol), copper powder (15 g, 236 mmol), zinc powder (3 g, 46 mmol), and 2.5 M aqueous sodium hydroxide (400 mL) was heated at reflux for 5 h and then cooled to ambient. The reaction mixture was filtered, and the filtrate was acidified with concentrated HCl. The precipitate was collected and washed with water, then dissolved and filtered. The filtrate was concentrated to deposit 2,4′-thiobis(benzoic acid), mass 50 g (81% of theory).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459263B2uspto-grants-2008_12