反应详情

A solution of Example 332B (8.0 g, 38.7 mmol) and p-toluenesulfonic acid (7.4 g, 38.7 mmol) in a mixture of water (20 mL) and acetone (85 mL) was refluxed for about 1 hour. The mixture was concentrated in vacuum, diluted with water and was neutralized by careful addition of potassium carbonate (2.7 g, 19.4 mmol). The precipitate was filtered off, washed with a minimum of water and diethyl ether and was dried in vacuum to give the above intermediate. MS (DCI/NH3): m/z 180 (M+NH4)+.

1. temperaturewas refluxed for about 1 hour
2. concentrationThe mixture was concentrated in vacuum
3. additiondiluted with water
4. filtrationThe precipitate was filtered off
5. washwashed with a minimum of water and diethyl ether
6. customwas dried in vacuum
7. customto give the above intermediate