反应详情

3,5-dimethyl-4-nitrophenol (33.43 g), methyl p-toluene sulfonate (40.97 g) and K2CO3 (31.79 g) are stirred at reflux in 200 ml of acetone for four and one half hours and then stirred at R.T. overnight. The reaction mixture is filtered to give a dark amber filtrate. The filtrate is concentrated in vacuo to a yellowish brown solid which is dissolved in ethyl acetate washed with saturated aqueous sodium chloride, dried and concentrated in vacuo. The concentrate is distilled (87°-104° C./0.10 mm) to give a yellow waxy looking solid. The solid is dissolved in hot ethanol and recrystallized, M.P. 50°-52° C.

1. filtrationThe reaction mixture is filtered
2. customto give a dark amber filtrate
3. concentrationThe filtrate is concentrated in vacuo to a yellowish brown solid which
4. dissolutionis dissolved in ethyl acetate
5. washwashed with saturated aqueous sodium chloride
6. customdried
7. concentrationconcentrated in vacuo
8. distillationThe concentrate is distilled (87°-104° C./0.10 mm)
9. customto give a yellow waxy
10. customrecrystallized