反应详情

A mixture of Example 1 (100 g at 100%) and chloracetonitrile (30.4 mL) in MeCN (500 mL) was heated at reflux for 2 h. The mixture was cooled, initially to 40° C. when water (300 mL) was added, and then to +10° C. The reaction was maintained at +10° C. for at least 1 h when the product was recovered by filtration. The filter cake was washed with cold (+10° C.) H2O (500 mL) followed by a cold (+10° C.) mixture of MeCN and H2O (1:1, 300 mL). The product was dried under vacuum at 50° C. to constant weight to give the title compound as an off-white solid (100.9 g). δH (DMSO-d6) 7.90 (1H, d, J 9.6 Hz), 7.46-7.33 (3H, m), 7.25 (2H, m), 6.95 (2H, br s), 6.35 (1H, d, J 9.6 Hz). LCMS (ES+) RT 2.69 minutes, 268 (M+H)+.

1. temperatureat reflux for 2 h
2. additionwas added
3. customto +10° C
4. temperatureThe reaction was maintained at +10° C. for at least 1 h when the product
5. filtrationwas recovered by filtration
6. washThe filter cake was washed with cold (+10° C.) H2O (500 mL)
7. additionfollowed by a cold (+10° C.) mixture of MeCN and H2O (1:1, 300 mL)
8. customThe product was dried under vacuum at 50° C. to constant weight