反应详情

The solution of 1.3 g (3.6 mmol) (R)-2-(3-bromo-benzyl)-morpholine-4-carboxylic acid tert-butyl ester in 80 mL diethyl ether was cooled down to −100° C. and treated dropwise with 2.6 mL (3.9 mmol; 1.5M solution in n-pentane) tert-butyllithium. After 15 min. 0.31 mL (4.0 mmol) N,N-dimethylformamide were added and the reaction stirred for another 1.5 h. The solution was poured on 10% aqueous ammonium chloride solution and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was chromatographed on silica gel with n-hexane:ethyl acetate (2:1 v/v) as eluant to give the desired compound as colorless oil (43%).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated
6. customThe residue was chromatographed on silica gel with n-hexane:ethyl acetate (2:1 v/v) as eluant