反应详情

This compound (V) (3.3 g, 10 mmols) was dissolved in ethyl acetate (30 ml), followed by agitating the solution together with Pd/C (5%) (0.6 g) and triethylamine (1.0 g) in hydrogen atmosphere at room temperature for 3 hours, filtering off Pd/C, adding toluene (100 ml), washing the resulting fluid with 2N-hydrochloric acid (50 ml), washing it with water till the washing water became pH 7, drying the toluene phase over anhydrous magnesium sulfate, filtering off magnesium sulfate, concentrating under reduced pressure to obtain white crystals and recrystallizing the crystals from methanol to obtain ethyl-2-(4-butyloxyphenyl)-5-pyrimidinecarboxylate (VI) (2.4 g) (yield: 80%) having a melting point 99.1° C.

1. filtrationfiltering off Pd/C
2. additionadding toluene (100 ml)
3. washwashing the resulting fluid with 2N-hydrochloric acid (50 ml)
4. washwashing it with water till the washing water
5. dry with materialdrying the toluene phase over anhydrous magnesium sulfate
6. filtrationfiltering off magnesium sulfate
7. concentrationconcentrating under reduced pressure
8. customto obtain white crystals
9. customrecrystallizing the crystals from methanol