反应详情

A mixture of the product of Example 8b (0.177 g, 1.19 mmol) and phosphorus oxychloride (3 mL) was heated under reflux for 30 min and then cooled to room temperature. The reaction mixture was poured over ice, taken to pH 8 by the addition of 1N aqueous sodium hydroxide solution, and extracted with dichloromethane (3×30 mL). The combined organic phase was dried over anhydrous magnesium sulfate, filtered, and evaporated under reduced pressure to provide the title compound (0.170 g, 88% yield).

1. temperaturewas heated
2. temperatureunder reflux for 30 min
3. additionThe reaction mixture was poured over ice
4. extractionextracted with dichloromethane (3×30 mL)
5. dry with materialThe combined organic phase was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customevaporated under reduced pressure