反应详情

To the product of step (e) (2.6 g) in glacial acetic acid (20 mls) was added concentrated hydrochloric acid (5.2 mls) and the whole was heated on a steam bath for three hours, during which time a solid slowly crystallised out of solution. The reaction mixture was cooled to room temperature and the crystallised solid was filtered off, washed thrice with glacial acetic acid and twice with diethyl ether. The resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours, affording 0.8 g of the sub-title compound. N.M.R. Spectroscopy confirmed the structure.

1. temperaturethe whole was heated on a steam bath for three hours, during which time a solid
2. customslowly crystallised out of solution
3. filtrationthe crystallised solid was filtered off
4. washwashed thrice with glacial acetic acid
5. dry with materialThe resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours