反应详情

Into a four-neck flask having an inner volume of 300 ml and equipped with a reflux condenser, a stirrer, a thermometer, and a nitrogen inlet were charged 16.0 g (0.10 mol) of 1,3-adamantanediol, 9.0 g (0.05 mol) of p-toluenesulfonic acid monohydrate, and 20 ml of 1,2-dimethoxyethane. After the atmosphere was displaced by nitrogen, 83.8 g (0.76 mol) of resorcinol was added. The mixture in the flask was placed in an oil bath at 90° C. and agitated for 6 hours. The mixture was cooled, added with 200 ml of pure water, agitated for 30 minutes, and then filtered to obtain a solid material. The material was dried under reduced pressure, then recrystallized from a methanol/water mixture solution. The crystals obtained were collected with washing by toluene, and then dried under reduced pressure until constant weight to obtain the target compound (yield 85%).

1. customInto a four-neck flask having
2. customan inner volume of 300 ml and equipped with a reflux condenser, a stirrer
3. additionwas added
4. customThe mixture in the flask was placed in an oil bath at 90° C.
5. temperatureThe mixture was cooled
6. stirringagitated for 30 minutes
7. filtrationfiltered
8. customto obtain a solid material
9. customThe material was dried under reduced pressure
10. customrecrystallized from a methanol/water mixture solution
11. customThe crystals obtained
12. customwere collected
13. washwith washing by toluene
14. customdried under reduced pressure until constant weight