HRID2252761

反应详情

EQUATION

反应方程式

HRID 2252761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 80 mg (0.19 mmol) 2-chloro-N-{4-[4-((R)-1-phenyl-ethylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzyl}-acetamide in 1.5 ml n-butanol is treated with 47 μl (0.48 mmol) piperidine and then heated to 100° C. for 2 h. The clear solution is cooled and the solvent evaporated. The residue is purified with flash chromatography using a mixture of ethyl acetate/methanol with increasing concentrations of methanol starting with 100:2.5 and ending with 10:1. The title compound is obtained as a colorless powder; m.p. 194-196° C.; MS-ES+: (M+H)+=469.

WORKUP

后处理

  1. temperatureThe clear solution is cooled
  2. customthe solvent evaporated
  3. customThe residue is purified with flash chromatography
  4. additiona mixture of ethyl acetate/methanol
  5. temperaturewith increasing concentrations of methanol starting with 100:2.5