HRID2071642

反应详情

EQUATION

反应方程式

HRID 2071642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.6 g. of 4-chloro-2-methyl-6-phenyl-2H-pyrazolo-[3,4-b]pyridine (0.06 mol.) and a solution of 100 ml. of methylpropylamine in 150 ml. of benzene are heated at 220° in an autoclave for 20 hours. After cooling, the mixture is evaporated in vacuo, and to the residue 100 ml. of water and 100 ml. of chloroform are added. After agitation, the chloroform extract is separated and dried with Na2SO4. Evaporation yields an oily product which, after treatment with ether, becomes solid. 14.3 g. of 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151°), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe mixture is evaporated in vacuo
  3. additionof chloroform are added
  4. extractionAfter agitation, the chloroform extract
  5. customis separated
  6. dry with materialdried with Na2SO4
  7. customEvaporation
  8. customyields an oily product which
  9. customof 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151°), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°