反应详情

To 16.1 grams 6-tert.-butyl-3-chloromethyl-2,4-dimethylphenol dissolved in 40 ml. of dry n-heptane was added 9.55 grams of trimethyl phosphite. One-third of the trimethyl phosphite was initially added dropwise at room temperature, the remainder being added dropwise at 70°. The reaction mixture was then heated at reflux (97°) for ten hours and the residual white solid isolated by stripping off the volatiles by distillation at 50° to 60° at reduced pressure. The residue was triturated twice with petroleum ether and recrystallized, after clarification, from a solvent mixture of n-hexane and isopropanol yielding the desired product as white crystals melting at 146° to 148°. (compound 1)

1. additionthe remainder being added dropwise at 70°
2. temperatureThe reaction mixture was then heated
3. temperatureat reflux (97°) for ten hours
4. customthe residual white solid isolated
5. distillationby distillation at 50° to 60° at reduced pressure
6. customThe residue was triturated twice with petroleum ether
7. customrecrystallized
8. additionafter clarification, from a solvent mixture of n-hexane and isopropanol yielding the desired product as white crystals melting at 146° to 148°