反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
45 g (0.22 moles) of 2,4-dichloro-thieno[3,4-d]pyrimidine are suspended in 1800 ml of absolute ethyl alcohol. To the cooled mixture 28.5 g (0.48 moles) of isopropylamine are added drop by drop whilst agitating vigorously and maintaining the temperature at between 0° and 5°C. A clear solution is obtained which is agitated for a further hour at ambient temperature. The solution is concentrated, making sure that the temperature of the bath does not exceed 30°C. The syrupy residue is poured into iced water whilst agitating well. A yellow solid is formed which is drained off, washed with water and dried. 49 g of 2-chloro-4-isopropylamino-thieno[3,4-d]pyrimidine are obtained with a yield reaching 98% of theory. M.P. : 189°-191°C.
WORKUP
后处理
- temperaturemaintaining the temperature at between 0° and 5°C
- customA clear solution is obtained which
- stirringis agitated for a further hour at ambient temperature
- concentrationThe solution is concentrated
- customdoes not exceed 30°C
- additionThe syrupy residue is poured into iced water whilst
- stirringagitating well
- customA yellow solid is formed which
- washwashed with water
- customdried