反応 #2460300

反応方程式

4-iodobenzoic acid

thiosalicylic acid

→

2,4′-thiobis(benzoic acid)

溶媒

sodium hydroxide

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 5 h
3. 3
   温度cooled
4. 4
   ろ過The reaction mixture was filtered
5. 5
   その他The precipitate was collected
6. 6
   洗浄washed with water
7. 7
   workup.DISSOLUTIONdissolved
8. 8
   ろ過filtered
9. 9
   濃縮The filtrate was concentrated

実験手順

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).

出典