反应详情

Chlorotrimethylsilane (2.35 ml, 0.018 mol) is added to a cooled (ice bath) solution of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]-thieno[3,2-d]pyrimidine-7-carboxylic acid (4.5 g, 0.018 mol) in pyridine (35 ml) under nitrogen. The mixture is stirred at ice bath temperature for 1 hour and then allowed to warm at room temperature. N-chlorosuccinimide (2.44 g, 0.018 mol) is added and the mixture is heated at 95° C. for 20 minutes. The mixture is cooled, diluted with ice water (5 ml) and stirred for 15 minutes. The precipitate is filtered, washed with boiling acetone and dried to give the product (3.5 g.) mp 335° C. (dec).

1. temperaturethe mixture is heated at 95° C. for 20 minutes
2. temperatureThe mixture is cooled
3. stirringstirred for 15 minutes
4. filtrationThe precipitate is filtered
5. washwashed with boiling acetone
6. customdried
7. customto give the product (3.5 g.) mp 335° C. (dec)