反应详情

温度

85 °C

K2CO3 (29.3 g, 212 mmol) was dissolved in water (162 mL). 1-Propanol (150 mL) was added. A sol. of 2,6-dichloro-para-cresol (25 g, 141 mmol) in 1-propanol (150 mL) was added. Methanesulfonic acid 2-(4-bromo-phenoxy)-ethyl ester (41.6 g, 141 mmol) was added. The mixture was stirred at 85° C. for 6 h. The heating oil bath was removed, and water (330 mL) was added dropwise when the internal temperature had reached 78° C. The beige suspension was allowed to cool to rt. The mixture was filtered, and the precipitate was washed with water. Drying the precipitate under high vacuum at 30° C. for 48 h yielded the title compound (43 g, 81%). LC-MS: tR=1.15 min.

1. customThe heating oil bath was removed
2. additionwater (330 mL) was added dropwise when the internal temperature
3. customhad reached 78° C
4. temperatureto cool to rt
5. filtrationThe mixture was filtered
6. washthe precipitate was washed with water
7. customDrying the precipitate under high vacuum at 30° C. for 48 h