反应详情

温度

23 °C

To a round bottomed flask was loaded l-mi of DMSO and 5 ml dichloromethane. The mixture was cooled to −50˜−60° C. Then a mixture of l-mi oxallyl chloride and 2 ml dichloromethane was injected in into the flask all at once. The mixture was stirred at the same temperature for another 5 minutes. Then 0.218 grams of (5-Methyl-6,7,8,9-tetrahydro-[1,2,4]triazolo[1,5-a]quinazolin-2-yl)-methanol in 2 ml dichloromethane was added within 2 minutes. The mixture was stirred at −50˜−60° C. for fifteen minutes and 0.7 ml triethylamine was next added. After another five minutes the reaction media was warmed up to 23° C. and a mixture of 20 ml water and 200 ml dichloromethane was added. The organic layer was dried over magnesium sulfate. Filter off the drying agent and concentrate the filtrate yielded 0.216 grams of product (99%). MS: 217.1(M+H). H-NMR(CDCl3): δ 10.20(s, 1H), 3.23(m, 2H), 2.78 (m, 2H) 2.63 (s, 3H, CH3), 2.00 (m, 4H),

1. customTo a round bottomed flask was loaded
2. temperatureThe mixture was cooled to −50˜−60° C
3. stirringThe mixture was stirred at −50˜−60° C. for fifteen minutes
4. customAfter another five minutes the reaction media
5. additionwas added
6. dry with materialThe organic layer was dried over magnesium sulfate
7. filtrationFilter off the drying agent
8. concentrationconcentrate the filtrate