反应详情

温度

80 °C

To a mixture of 11E (2.6 g, 6.19 mmol) in MeCN (30 mL) was added ZnCl2 (1.27 g, 1.5 eq, 9.3 mmol) at room temperature, followed by AcOH (30 mL) and H3PO4 (30 mL) The reaction mixture was stirred 80° C. overnight. After reaction completed, the mixture was cooled and poured into crushed ice under stirring, neutralized to pH=7˜8, extracted with ethyl acetate, dried and concentrated to give 1.6 g of crude product, which was purified by column chromatography on silica gel to give 500 mg of pure product (11F).

1. customAfter reaction
2. temperaturethe mixture was cooled
3. additionpoured
4. custominto crushed ice
5. stirringunder stirring
6. extractionextracted with ethyl acetate
7. customdried
8. concentrationconcentrated
9. customto give 1.6 g of crude product, which
10. customwas purified by column chromatography on silica gel