反应详情

To a solution of 855 g of potassium hydroxide in 7 litres of water are added, at 50° C under argon, 420 g of thiophenol and the mixture is stirred for 15 minutes. There are then added thereto 22.1 g of copper powder and 1 kg of 2-iodo-5-methyl-benzoic acid and the mixture is heated for 7 hours under reflux. After cooling, the mixture is adjusted to pH 3 with 600 ml of concentrated hydrochloric acid and extracted with methylene chloride, washed with water, dried over sodium sulphate and concentrated to a thick crystal mash. This is filtered under suction, washed with cold ethanol and low-boiling petroleum ether and dried. There is obtained 3-methyl-6-(phenylthio)-benzoic acid of melting point 156°-157° C.

1. additionThere are then added
2. temperatureunder reflux
3. temperatureAfter cooling
4. extractionextracted with methylene chloride
5. washwashed with water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated to a thick crystal mash
8. filtrationThis is filtered under suction
9. washwashed with cold ethanol and low-boiling petroleum ether
10. customdried