反应详情

A solution of 1,4-dioxa-10-azadispiro[4.2.4.2]tetradecan-11-one (10.5 g, 49.8 mmol) in aq.HCl (2N, 20 mL) was stirred at RT for 2 h. The reaction mixture was then concentrated under reduced pressure and diluted with water. It was extracted with ethyl acetate (Three times) and the combined organic phases were washed with water, brine, dried over sodium sulfate, filtered and concentrated. Purification by flash chromatography on silica (Pet.Ether:EtOAc) afforded the title compound as a white solid (7.5 g, 92%). 1H NMR (400 MHz, DMSO-d6) δ 7.58 (m, 1H), 3.15-3.15 (s, 2H), 2.30 (s, 4H), 2.28-2.25 (m, 2H), 1.82-1.79 (m, 4H).

1. concentrationThe reaction mixture was then concentrated under reduced pressure
2. additiondiluted with water
3. extractionIt was extracted with ethyl acetate (Three times)
4. washthe combined organic phases were washed with water, brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by flash chromatography on silica (Pet.Ether:EtOAc)