反应详情

温度

75 °C

106 Parts of N,N-dimethylformamide were added dropwise to 650 parts of aluminum chloride and the solution was stirred for 15 min at 75° C. There were added portionwise 112 parts of 3,4-dihydro-2(1H)-quinazolinethione and, after stirring for 15 min at 75° C., 136 parts of 3-pyridinylcarbonyl chloride hydrochloride. Stirring at 75° C. was continued overnight and then the mixture was poured into 2500 parts of ice-water. The precipitate was filtered off and stirred for 13 hours in a mixture of ice-water and 1530 parts of a sodium hydroxide solution 50%. The product was filtered off, washed with water and dried, yielding 150 parts (82%) of (3-pyridinyl) (1,2,3,4-tetrahydro-2-thioxo-6-quinazolinyl)methanone; (decomp.) (interm. 54).

1. stirringafter stirring for 15 min at 75° C.
2. stirringStirring at 75° C.
3. waitwas continued overnight
4. filtrationThe precipitate was filtered off
5. stirringstirred for 13 hours in a mixture of ice-water and 1530 parts of a sodium hydroxide solution 50%
6. filtrationThe product was filtered off
7. washwashed with water
8. customdried