反应详情

Chlorotrimethylsilane (2.6 ml, 0.02 mol) is added to a cooled (icebath) solution of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxylic acid (5.0 g., 0.02 mol) in pyridine (40 ml) under nitrogen. The mixture is stirred at ice bath temperature for one hour and then allowed to warm to room temperature. N-Chlorosuccinimide (2.74 g., 0.02 mol) is added and the mixture is heated at 90°-95° C. for 20 minutes. The mixture is cooled, diluted with water (5 ml) and stirred for 15 minutes. The precipitate is filtered off, dried, washed with boiling acetone (3×100 ml) and recrystallized from dimethylformamide to give the product (3.9 g.), mp 320° C. (dec).

1. temperaturethe mixture is heated at 90°-95° C. for 20 minutes
2. temperatureThe mixture is cooled
3. stirringstirred for 15 minutes
4. filtrationThe precipitate is filtered off
5. customdried
6. washwashed with boiling acetone (3×100 ml)
7. customrecrystallized from dimethylformamide
8. customto give the product (3.9 g.), mp 320° C. (dec)