163169-10-6

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• Preparation

  Oxazoline (S)-3a (0.158 g, 0.53 mmol) was added to a flame-dried Schlenk tube under an argon atmosphere and dissolved in anhydrous diethyl ether (6 mL). Tetramethylethylenediamine (0.100 mL, 0.70 mmol) was added, followed by cooling the orange solution to -78 °C and stirring for 5 min. Then, sec-butyllithium (1.4 M) (0.500 mL, 0.70 mmol) was slowly added. After stirring for 2 hours, the mixture was heated to 0 °C and freshly distilled dichlorophosphine (0.120 mL, 0.70 mmol) was added via syringe. The reaction was allowed to rise to room temperature and then allowed to stand for another 10 min. The mixture was diluted with diethyl ether and then quenched with a saturated aqueous sodium bicarbonate solution. The organic matter was separated by water, dried over magnesium sulfate, and the solvent was removed under vacuum to give the crude product. Column chromatography (SiO2, 10% EtOAc in hexane solution) eluted the crude product as an orange solid diastereomer (0.11 g, 43%).;

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