反应详情

To a solution of methyl 2-(2-thienyl)-5-benzoxazolecarboxylate (1.50 g) in tetrahydrofuran (30 ml) was slowly added lithium aluminum hydride (220 mg) at 0° C., stirred for 30 minutes. To the reaction mixture was added water, which was made acidic with 1N-hydrochloric acid, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography. From the fraction eluted with ethyl acetate-hexane (4:1, v/v), 2-(2-thienyl)-5-benzoxazolyl methanol (1.03 g, 77%) was obtained. The recrystalization from ethyl acetate-hexane gave colorless needles, mp 158-159° C.

1. customat 0° C.
2. extractionextracted with ethyl acetate
3. washThe ethyl acetate layer was washed with water
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. washFrom the fraction eluted with ethyl acetate-hexane (4:1