反应详情

50 mL of a tetrahydrofuran (THF) solution containing 10.00 g (0.049 mol) of 2,6-di-tert-butylphenol were dropped into 100 mL of a THF suspension of 2.03 g (0.051 mol) of 60% oil-dispersed sodium hydride at 0° C. followed by stirring for 1 hour at the same temperature to prepare sodium 2,6-di-tertbutylphenoxide. 5.81 g (0.051 mol) of 1,3-dimethyl-2-imidazolidinone were added to this solution, and after stirring for 30 minutes at 0° C., 5.83 g (0.051 mol) of methanesulfonyl chloride were dropped in followed by stirring for 2 hours at 25° C. The reaction liquid was placed in 30% aqueous hydrochloric acid solution and following separation of the organic layer, the organic layer was washed once with 1 N aqueous NaOH solution and twice with water followed by drying with MgSO4 and concentrating. The resulting crude crystals were purified by crystallization with a 1/1 (volumetric ratio) mixture of n-hexane and isopropanol to obtain 4.8 g (yield: 35%) of 2,6-di-tert-butylphenyl methanesulfonate (white crystals, melting point: 83° C.).

1. stirringafter stirring for 30 minutes at 0° C.
2. stirringby stirring for 2 hours at 25° C
3. customThe reaction liquid
4. customseparation of the organic layer
5. washthe organic layer was washed once with 1 N aqueous NaOH solution and twice with water
6. dry with materialby drying with MgSO4
7. concentrationconcentrating
8. customThe resulting crude crystals were purified by crystallization with a 1/1 (volumetric ratio) mixture of n-hexane and isopropanol