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温度

0 °C

(3RS,4RS)-3,4-diethylazetidin-2-one (step 2) (100 mg, 0.786 mmol) in dry THF (5 ml) was cooled to −78° C. and was treated with lithium bis(trimethylsilyl)amide (0.786 ml, 0.786 mmol) [1M in THF]. The solution was allowed to warm to 0° C. then re-cooled to 0° C. before adding bromoacetonitrile (0.060 ml, 0.865 mmol). The mixture was allowed to warm to RT overnight. 10% Aqueous citric acid (30 ml) was added and the mixture was extracted with ether (4×40 ml). The combined organic layers were dried MgSO4, filtered and evaporated to dryness. Purification by chromatography on silica eluting with 0-100% Et2O in iso-hexane afforded the title compound;

1. temperaturethen re-cooled to 0° C.
2. temperatureto warm to RT overnight
3. extractionthe mixture was extracted with ether (4×40 ml)
4. filtrationfiltered
5. customevaporated to dryness
6. customPurification by chromatography on silica eluting with 0-100% Et2O in iso-hexane