反应详情

温度

0 °C

To a solution of 0.204 g (0.0053 mol) of lithium aluminum hydride suspended in 20 mL THF was added dropwise 1.0 g (0.0053 mol) of the product from step C dissolved in 10 mL THF. The dark reaction mixture was refluxed for 1 hour, cooled to 0° C. and 50 mL of a saturated solution of ammonium chloride was added. The reaction was extracted with ethyl acetate (3×50 mL), washed with brine (1×100 mL), dried over anhydrous magnesium sulfate, filtered into a flask and added 1.0 g (0.0053 mol) α,α,α-trifluoro-p-tolylisocyanate all at once. The reaction was stirred for 0.5 hours, concentrated under vacuum and chromatographed using 30% ethyl acetate/70% hexanes as eluent to afford 0.250 g of a purple solid, mp 136°-138° C.

1. customThe dark reaction mixture
2. temperaturewas refluxed for 1 hour
3. extractionThe reaction was extracted with ethyl acetate (3×50 mL)
4. washwashed with brine (1×100 mL)
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered into a flask
7. concentrationconcentrated under vacuum
8. customchromatographed