反应详情

To a solution of 2-[(3,3-dimethyl-2,3-dihydro-1-benzofuran-4-yl)oxy]-5-nitropyrimidine (Intermediate 64, 1.257 g) in a mixture tetrahydrofuran/water (30 ml/15.00 ml) iron (1.222 g, 21.88 mmol) and ammonium chloride (1.170 g, 21.88 mmol) were added. The reaction mixture was stirred at room temperature for 48 hours. The catalyst was filtered off, and the filtrate was extracted with ethyl acetate (3×50 ml). The combined organic layers were dried over sodium sulphate, filtered and evaporated. The residue was recrystallized from ethyl acetate to afford the title compound (768 mg) as a white solid.

1. filtrationThe catalyst was filtered off
2. extractionthe filtrate was extracted with ethyl acetate (3×50 ml)
3. dry with materialThe combined organic layers were dried over sodium sulphate
4. filtrationfiltered
5. customevaporated
6. customThe residue was recrystallized from ethyl acetate