反应详情

A mixture of Example 1A (15.9 g, 49.6 mmol) in POCl3 (55 ml, 590 mmol) and diisopropylethylamine (55 ml, 315 mmol) was heated at 90° C. for 1.5 hours. The reaction mixture was concentrated. The residue was treated with ice and saturated NaHCO3 carefully and then extracted with ethyl acetate. The insoluble material suspended in the two layers was filtered, washed with ether and water, and oven dried to provide the title compound. The two layers in the filtrate were separated. The aqueous layer was washed with ethyl acetate. The combined organic layers were dried over MgSO4, filtered, concentrated, and triturated (twice) with ethyl acetate/ether to provide additional title compound.

1. concentrationThe reaction mixture was concentrated
2. additionThe residue was treated with ice and saturated NaHCO3 carefully
3. extractionextracted with ethyl acetate
4. filtrationwas filtered
5. washwashed with ether and water, and oven
6. customdried