反应详情

To a solution of 3-{2-[1-(4-bromo-phenyl)-ethylamino]-ethyl}-2-methyl-hex-5-en-3-ol (2.2 g, crude) and TEA (4 eq) in dried CH2Cl2 (60 mL) at 0° C. was added triphosgene (2.12 g, 7.12 mmol). The mixture was stirred at rt till the reaction was over. Water was added, and the layers were separated. The aqueous layer was extracted with CH2Cl2. The combined organic phase was washed with water, dried over Na2SO4, and condensed to give the crude product, which was purified by column to give 6-allyl-3-[1-(4-bromo-phenyl)-ethyl]-6-isopropyl-[1,3]oxazinan-2-one (500 mg, crude).

1. customthe layers were separated
2. extractionThe aqueous layer was extracted with CH2Cl2
3. washThe combined organic phase was washed with water
4. dry with materialdried over Na2SO4, and condensed
5. customto give the crude product, which
6. customwas purified by column