反应详情

8-thia-4,5-diazatricyclo[7.4.0.02,7]trideca-1(9),2(7),3-trien-6-one was prepared following the procedures of U.S. Pat. No. 8,716,274, Example 191d and converted to (4-fluoro-2-{6-oxo-8-thia-4,5-diazatricyclo[7.4.0.02,7]trideca-1(9),2(7),3-triene-5-yl}-6-(bromo)phenyl)carbinol 108a. To a mixture of 108a (4.1 g, 10 mmol) and Et3N (1.95 mL, 14 mmol) in THF (50 mL) was added AcCl (0.85 mL, 12 mmol). The mixture was stirred at rt for 1 h, diluted with water and extracted with EA. The combined organic layers were dried over Na2SO4, filtered and concentrated to give compound 108b (4.0 g) as yellow solid. MS-ESI: [M+H]+ 451.0

1. extractionextracted with EA
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated