反应详情

温度

60 °C

Powdered anhydrous aluminum chloride (3.0 g, 22.5 mmol) was dissolved in anhydrous nitrobenzene (10 mL) at 100° C. The solution was cooled and 2-methoxyphenyl propionate (2.0 g, 11.1 mmol) was added rapidly. The reaction mixture was heated at 60° C. for 1.5 h and cooled, 3 N NaOH was added, and the mixture was stirred for 15 min. The suspension was filtered off, washed with water. The filtrate was then washed with CH2Cl2 twice, acidified with 3 N HCl, extracted with CH2Cl2. The extract was dried, concentrated, and purified by column chromatography (petroleum ether/EtOAc=10/1 to 5/1) to give the desired product (874 mg, 44% yield) as a yellow oil.

1. temperatureThe solution was cooled
2. temperaturecooled
3. filtrationThe suspension was filtered off
4. washwashed with water
5. washThe filtrate was then washed with CH2Cl2 twice
6. extractionextracted with CH2Cl2
7. customThe extract was dried
8. concentrationconcentrated
9. custompurified by column chromatography (petroleum ether/EtOAc=10/1 to 5/1)