반응 #2460298

반응 방정식

thiosalicylic acid

3-iodoanisole

potassium carbonate

→

2-(3-methoxyphenylthio)benzoic acid

용매

N-methylpyrrolidinone

반응 조건

후처리

1. 1
   기타by sparging with nitrogen for 10 min
2. 2
   온도cooled
3. 3
   workup.ADDITIONThe reaction mixture was poured onto a mixture of 500 g of ice plus 40 mL of concentrated HCl
4. 4
   기타The resulting precipitate was collected
5. 5
   세척washed with water
6. 6
   기타dried
7. 7
   workup.DISSOLUTIONThe precipitate was dissolved in acetone
8. 8
   여과filtered through Celite
9. 9
   농축concentrated
10. 10
    기타The product was purified by recrystallization from aqueous ethanol
11. 11
    기타A tan powder was obtained

실험 절차

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).

출처