| tangyyer |
2009-06-29 07:40 |
Nitrogen atmosphere bottom, at -20℃, mixture of N,N,N'-Trimethylethylenediamine (2.86g) and THF(80 mL) , n-butylithium 2.6M solution, and 2-(Triisopropylsilyl)oxazole-5-carboxaldehyde [CAS No .869542-45-0] (5.08g) was sequentially added dropwisely. After 3 hours of stirring at -20 ℃, more n-butylithium 2.6M solution (8.46mL) was added dropwisely. After 3 hours of stirring at -20 ℃, the reaction mixture was cooled to -75℃, 2-bromo-1,1,1,2-tetrafluoroethane (7.12mL) (这个好像不是很准确，但没有合适的翻译）was added. After returning to room temperature, ethyl acetate (300mL) and ammonium chloride water solution (300mL) was added to the reaction mixture, extracted and dried with MgSO4, and filtered and the filtrate was evaporated under vacuum to obtaine the crude product. Silicagel column chromatography (a mixture of EA-butane) the crude product and got a pure compound (1.94g) as brown liquid.
先翻译第一段，hope helpful! |
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