反应详情

温度

170 °C

12.1 g (0.1 mol) of formanilide, 22.1 g (0.11 mol) of 2-bromo-5-methoxytoluene of the formula (101), 13.8 g (0.1 mol) of anhydrous potassium carbonate, 2.0 g (0.0079 mol) of iodine and 1.6 g (0.025 mol) of copper powder are initially placed in a 100 ml sulfonating flask fitted with an anchor stirrer, thermometer, condenser and oil bath, and the mixture is stirred. It is heated to 170° C. and then stirred at 170° C. for 22 hours, to give a black melt. This melt is then cooled to 80° C., a little toluene is added, and the solution is filtered. The residue is rinsed with toluene. The toluene filtrate is distilled with steam spray (distillate: water/toluene/unreacted 2-bromo-5-methoxytoluene) to leave a residue which comprises a mixture of black oil and water. The black oil is boiled under reflux for 25 hours with 250 g of 50% potassium hydroxide solution. The product obtained is extracted with toluene and washed with hot water. The toluene phase is dried over sodium sulfate, filtered and concentrated. The residue which remains comprises 17.0 g of the compound of the formula ##STR12## as black crystals.

1. customfitted with an anchor stirrer
2. stirringstirred at 170° C. for 22 hours
3. customto give a black melt
4. temperatureThis melt is then cooled to 80° C.
5. filtrationthe solution is filtered
6. washThe residue is rinsed with toluene
7. distillationThe toluene filtrate is distilled with steam spray (distillate: water/toluene/unreacted 2-bromo-5-methoxytoluene)
8. customto leave a residue which
9. customThe product obtained
10. extractionis extracted with toluene
11. washwashed with hot water
12. dry with materialThe toluene phase is dried over sodium sulfate
13. filtrationfiltered
14. concentrationconcentrated