HRID1579421

反应详情

EQUATION

反应方程式

HRID 1579421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturemaintaining the temperature at between 0° and 5°C
  2. customA clear solution is obtained which
  3. stirringis agitated for a further hour at ambient temperature
  4. concentrationThe solution is concentrated
  5. customdoes not exceed 30°C
  6. additionThe syrupy residue is poured into iced water whilst
  7. stirringagitating well
  8. customA yellow solid is formed which
  9. washwashed with water
  10. customdried