反应详情

According to (16-1) described in Reference Example 16, 659 mg (3.80 mmol) of tert-butyl N-(allyloxy)carbamate prepared from tert-butyl N-hydroxycarbamate, sodium hydride and allyl bromide was dissolved in 10 ml of dichloromethane, and the thus prepared solution was mixed with 886 mg (4.67 mmol) of m-chloroperbenzoic acid and stirred at room temperature for 24 hours. The reaction solution was filtered, mixed with a 1 N sodium hydroxide aqueous solution and extracted with chloroform. The chloroform layer was washed with saturated brine and dried with anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1) to obtain 447 mg (yield, 62%) of tert-butyl N-(2,3-epoxypropoxy)carbamate.

1. filtrationThe reaction solution was filtered
2. additionmixed with a 1 N sodium hydroxide aqueous solution
3. extractionextracted with chloroform
4. washThe chloroform layer was washed with saturated brine
5. dry with materialdried with anhydrous sodium sulfate
6. customthe solvent was evaporated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1)