反应详情

9A (3.5 g, 9.28 mmol) was added to MeCN (50 mL) and stirred at room temperature. To the mixture was added ZnCl2 (1.91 g, 13.93 mmol, 1.5 eq), followed by AcOH (50 mL) and H3PO4 (50 mL) The reaction mixture was heated to 80° C. and stirred 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 2.4 g of product (9B).

1. temperaturewas heated to 80° C.
2. stirringstirred overnight
3. customAfter reaction
4. temperaturethe mixture was cooled
5. additionpoured
6. custominto crushed ice
7. stirringunder stirring
8. extractionextracted with ethyl acetate
9. customdried
10. concentrationconcentrated