反应详情

The compound obtained in (d) above (6.58 g; 17.6 mmoles) was dissolved in tetrahydrofuran (50 mL), treated with carbonyldiimidazole (3.1 g; 19.1 mmoles), and stirred for 1 hour at room temperature under an atmosphere of N2 . A solution of 2,4,6-trimethoxyaniline (3.2 g; 17.6 mmoles/50 mL THF) was then added in one portion and the solution was stirred at room temperature for overnight. Ethyl acetate (150 mL) was then added as well as aqueous HCl (1N). The layers were separated and the organic portion was washed with NaOH (1N), brine, and then dried over MgSO4. The drying agent was filtered and the filtrate concentrated in vacuo leaving a lavender colored solid which was purified by silica gel chromatography using chloroform (95%)/methanol (5%) as the eluent. Yield: 6.7 g (70%), mp 119°-120° C.

1. stirringthe solution was stirred at room temperature for overnight
2. customThe layers were separated
3. washthe organic portion was washed with NaOH (1N), brine
4. dry with materialdried over MgSO4
5. filtrationThe drying agent was filtered
6. concentrationthe filtrate concentrated in vacuo
7. customleaving a lavender colored solid which
8. customwas purified by silica gel chromatography