HRID75299

反应详情

EQUATION

反应方程式

HRID 75299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (S)-1-(1-methyl-6-(3-methyl-1H-pyrazol-4-yl)-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine dihydrochloride (200 mg, 0.609 mmol), 4-chloro-6-methyl-2-(methylthio)pyrimidine-5-carbonitrile (182 mg, 0.914 mmol), and N-ethyl-N-isopropylpropan-2-amine (0.318 mL, 1.83 mmol) in acetonitrile (5 mL) was heated in a microwave reactor at 120° C. for 2 hours. The mixture was then concentrated. The residue was dissolved in MeOH/DCM, absorbed onto silica gel, and purified by column chromatography eluting with 20-80% EtOAc in hexane over 60 minutes to give the title compound. ESI-MS m/z [M+H]+ calc'd for C21H22N8S, 419; found 419.

WORKUP

后处理

  1. concentrationThe mixture was then concentrated
  2. dissolutionThe residue was dissolved in MeOH/DCM
  3. customabsorbed onto silica gel
  4. custompurified by column chromatography
  5. washeluting with 20-80% EtOAc in hexane over 60 minutes