反应详情

温度

105 °C

A mixture of 3,4,5-trimethoxytoluene (9.11 g; 50 mmol), octane (25 ml) and iron(III)chloride (50 mg) is stirred at 105° C., and percolating nitrogene 2,6-dichlorobenzoylchloride (12.04 g; 57.5 mmol) is added dropwise within 15 minutes. The mixture is kept at 105° C. and stirred for another 15 minutes. After cooling to 50° C. ethylacetate (50 ml) is added, the mixture shaken twice with 2N hydrochloric acid, once with water and dried. The ethylacetate is evaporated (70° C.) and the liquid cooled with stirring. At 50° C. petrolether (50 ml) is added. The white crystals formed are sucked off, washed with petrolether and dried. Yield 12.55 g (70.7%), mp. 92° C.

1. additionis added dropwise within 15 minutes
2. customis kept at 105° C.
3. stirringstirred for another 15 minutes
4. additionis added
5. customdried
6. customThe ethylacetate is evaporated (70° C.)
7. temperaturethe liquid cooled
8. stirringwith stirring
9. additionAt 50° C. petrolether (50 ml) is added
10. customThe white crystals formed
11. washwashed with petrolether
12. customdried