反应详情

Phloroglucinol (35.1 g, 279 mmol) was dissolved into ethyl ether (500 mL) solution, followed by zinc chloride (8 g, 59 mmol) and 2-methoxy acetonitrile (18 g, 253 mmol) added in the solution under ice water bath condition. Dry HCl gas was bubbled into the reaction mixture, vigorously stirring for 5 hours, and precipitate was formed. The precipitate was filtered and collected, followed by dissolved into water and refluxed for 3 hours. After cooling, pink precipitate was collected, and desired white compound can be obtained after recrystallization with water. (45 g, yield 81%) 1HNMR (400 MHz, DMSO-d6): δ=12.14 (s, 2H), 10.41 (s, 1H), 5.79 (s, 2H), 4.56 (s, 2H), 3.32 (s, 3H).

1. additionadded in the solution under ice water bath condition
2. customDry HCl gas was bubbled into the reaction mixture
3. customprecipitate was formed
4. filtrationThe precipitate was filtered
5. customcollected
6. dissolutionby dissolved into water
7. temperaturerefluxed for 3 hours
8. temperatureAfter cooling
9. custompink precipitate was collected
10. customdesired white compound can be obtained
11. customafter recrystallization with water