反应 #2460298

反应方程式

thiosalicylic acid

3-iodoanisole

potassium carbonate

→

2-(3-methoxyphenylthio)benzoic acid

溶剂

N-methylpyrrolidinone

反应条件

后处理

1. 1
   其他by sparging with nitrogen for 10 min
2. 2
   温度cooled
3. 3
   workup.ADDITIONThe reaction mixture was poured onto a mixture of 500 g of ice plus 40 mL of concentrated HCl
4. 4
   其他The resulting precipitate was collected
5. 5
   洗涤washed with water
6. 6
   其他dried
7. 7
   workup.DISSOLUTIONThe precipitate was dissolved in acetone
8. 8
   过滤filtered through Celite
9. 9
   浓缩concentrated
10. 10
    其他The product was purified by recrystallization from aqueous ethanol
11. 11
    其他A tan powder was obtained

实验过程

First, 2-(3-methoxyphenylthio)benzoic acid was prepared. A stirred mixture of thiosalicylic acid (3.57 g, 23 mmol), 3-iodoanisole (5.42 g, 23 mmol), potassium carbonate (7.04 g, 51 mmol), copper powder (0.29 g, 5 mmol), and N-methylpyrrolidinone (75 mL) was deaerated by sparging with nitrogen for 10 min, heated at 165° C. for 2 h, and then cooled to ambient. The reaction mixture was poured onto a mixture of 500 g of ice plus 40 mL of concentrated HCl. The resulting precipitate was collected, washed with water, and dried. The precipitate was dissolved in acetone and filtered through Celite, then concentrated to deposit a crude product. The product was purified by recrystallization from aqueous ethanol. A tan powder was obtained, mass: 4.60 g (76% of theory).

来源