反应详情

The product of Example 90E (0.245 g, 0.356 mmol) in 1,4-dioxane (3 mL), was treated with a solution of lithium hydroxide monohydrate (0.0747 g, 1.78 mmol) in water (1.5 mL) at room temperature, the resulting mixture was heated at 60° for 25 minutes. The reaction mixture was cooled, diluted with water (10 mL), adjusted the pH to 3 with 1N aqueous HCl, and the resulting precipitate was collected by vacuum filtration. Washing of the crude product with small volumes of 1,4-dioxane afforded the title compound (0.113 g, 0.258 mmol, 72%). MS (ESI+) m/z 438 (M+H)+, MS (ESI−) m/z 436 (M−H)−.

1. temperaturethe resulting mixture was heated at 60° for 25 minutes
2. temperatureThe reaction mixture was cooled
3. filtrationthe resulting precipitate was collected by vacuum filtration
4. washWashing of the crude product with small volumes of 1,4-dioxane