反应详情

A solution of ethyl 2-(2,5,6-trimethylbenzimidazol-1-yl)acetate (6.15 g) in dry tetrahydrofuran (20 ml) was added to a suspension of lithium aluminium hydride (0.95 g) was dry tetrahydrofuran (60 ml) at 0° C. The reaction was allowed to warm to room temperature and stirred at room temperature for 1 hour. Water (1 ml) was added dropwise to the reaction followed by 15% sodium hydroxide (3 ml) and water (3 ml). The suspension was filtered and the solvent removed under reduced pressure. The product was dissolved in dichloromethane, dried over magnesium sulphate and the solvent removed under reduced pressure. The residue was triturated with acetone, the solid filtered and dried under reduced pressure to yield the title compound (1.9 g, 37%), m.p. 191°-2° C. Found: C, 70.17; H, 8.07; N, 13.56. C12H16N2O requires: C, 70.59; H, 7.84; N, 13.72%.

1. customat 0° C
2. filtrationThe suspension was filtered
3. customthe solvent removed under reduced pressure
4. dissolutionThe product was dissolved in dichloromethane
5. dry with materialdried over magnesium sulphate
6. customthe solvent removed under reduced pressure
7. customThe residue was triturated with acetone
8. filtrationthe solid filtered
9. customdried under reduced pressure