反应详情

The product of Example 5F (123 mg, 0.6332 mmol) and phosphorous oxychloride (2 mL) were refluxed for 1 hour under a nitrogen atmosphere. The solution was cooled in an ice bath, treated with ice, and the pH adjusted to 7 with 6N aqueous sodium hydroxide. Extracted with methylene chloride (3×50 mL) and dried the combined organic extracts over anhydrous sodium sulfate, filtered and concentrated under vacuum giving the title compound as a brown oil (120 mg, 0.564 mmol, 89%).

1. temperatureThe solution was cooled in an ice bath
2. additiontreated with ice
3. extractionExtracted with methylene chloride (3×50 mL)
4. dry with materialdried the combined organic extracts over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum