反应 #2460300
ord-e4077168dc75468aa1950b9c830a5b79
反应方程式
4-iodobenzoic acid
thiosalicylic acid
→
2,4′-thiobis(benzoic acid)
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度was heated
- 2温度at reflux for 5 h
- 3温度cooled
- 4过滤The reaction mixture was filtered
- 5其他The precipitate was collected
- 6洗涤washed with water
- 7workup.DISSOLUTIONdissolved
- 8过滤filtered
- 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).