反应详情

温度

100 °C

Concentrated hydrochloric acid (200 ml) was added to a suspension of the product of Example 4 Step 1 (20 g, 93 mmol) in water (120 ml). The mixture was heated at 100° C. for 60 hours, cooled to room temperature and the solvent concentrated in vacuo. The residue was azeotroped with toluene (×5) and dried over phosphorus pentoxide. The resulting solid was triturated with diethyl ether and acetone to yield the title compound (14.0 g, 81%); MS (ES−) m/e 186 [M−H]−.

1. temperaturecooled to room temperature
2. concentrationthe solvent concentrated in vacuo
3. customThe residue was azeotroped with toluene (×5)
4. dry with materialdried over phosphorus pentoxide
5. customThe resulting solid was triturated with diethyl ether and acetone