HRID1046531

反应详情

EQUATION

反应方程式

HRID 1046531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-{4-[8-(1-hydroxy-1-methyl-ethyl)-imidazo[1,2-a]pyridin-3-yl]-pyrimidin-2-ylamino}-cyclohexanecarboxylic acid (0.175 g), BOP (0.39 g), DIEA (0.23 mL), and piperidin-4-ol (67 mg) in DMF (5 mL) was stirred at RT overnight. The resulting solid was filtered and dried, purified by ISCO using 100% DCM to 20% MeOH/DCM. The fractions were collected and concentrated, then titurated with EtOAc, and the resulting solid filtered and dried at 50° C. overnight to provide (4-{4-[8-(1-hydroxy-1-methyl-ethyl)-imidazo[1,2-a]pyridin-3-yl]-pyrimidin-2-ylamino}-cyclohexyl)-(4-hydroxy-piperidin-1-yl)-methanone (Compound 2, 140.4 mg). Mp=188.0-190.0° C.

WORKUP

后处理

  1. filtrationThe resulting solid was filtered
  2. customdried
  3. custompurified by ISCO
  4. customThe fractions were collected
  5. concentrationconcentrated
  6. filtrationthe resulting solid filtered
  7. customdried at 50° C. overnight