反应详情

Chlorotrimethylsilane (0.4 ml, 0.03 mol) is added to a cooled (ice bath) solution of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxylic acid (0.75 g., 0.03 mol) in pyridine (5 ml) under nitrogen. The mixture is stirred at ice bath temperature for one hour and then allowed to warm to room temperature. N-Chlorosuccinimide (0.8 g., 0.06 mol) is added and the mixture is heated at 95° C. for 20 minutes. The mixture is cooled, diluted with water (3 ml) and stirred for 15 minutes. The precipitate is filtered off, dried and recrystallized from ethanol to give the product (0.5 g.), mp 285° 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 off
5. customdried
6. customrecrystallized from ethanol
7. customto give the product (0.5 g.), mp 285° C. (dec)