反应详情

温度

75 °C

Methyl N-(4-chloro-5-cyclopentyloxy-2-fluorophenyl)carbamate (2.87 g, 10 mmol), ethyl 2-hydroxy-3-methyl-3-butenoate (4.32 g, 30 mmol), ferric chloride (162 mg, 1.0 mmol) and tributylamine (92.7 mg, 0.5 mmol) were introduced into a flask (25 cc) equipped with a distillation unit, and the reaction was conducted at 200° C. for 3 hours. After completion of the reaction, the reaction solution was allowed to cool to 70 to 80° C., and a mixed solution consisting of methanol (5 mL) and 6N hydrochloric acid (0.25 mL) was added thereto and mixed homogeneously. Then, the reaction solution was left to stand at room temperature. The precipitated solid was collected by filtration, washed with a mixed solution consisting of methanol (8 mL) and 6N hydrochloric acid (0.8 mL) and then water (10 mL) and dried completely under reduced pressure to obtain 3-(4-chloro-5-cyclopentyloxy-2-fluorophenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (1.93 g, yield 54.5%).

1. customequipped with a distillation unit
2. customAfter completion of the reaction
3. additionwas added
4. additionmixed homogeneously
5. waitThen, the reaction solution was left
6. customto stand at room temperature
7. filtrationThe precipitated solid was collected by filtration
8. washwashed with a mixed solution
9. dry with materialwater (10 mL) and dried completely under reduced pressure