HRID75297

反应详情

EQUATION

反应方程式

HRID 75297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

(S)-1-(1-methyl-6-(thiazol-4-yl)-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine dihydrochloride (200 mg, 0.604 mmol), 4-amino-6-chloro-2-(methylthio)pyrimidine-5-carbonitrile (182 mg, 0.906 mmol), and N-ethyl-N-isopropylpropan-2-amine (0.315 mL, 1.81 mmol) were combined in acetonitrile (6 mL). The reaction mixture was heated in a microwave reactor at 120° C. for 2 hours and 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. The fractions containing the desired product were collected and concentrated to give the title compound (22 mg, 9%). ESI-MS m/z [M+H]+ calc'd for C19H18N8S2, 423; found 423.

WORKUP

后处理

  1. concentrationconcentrated
  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
  6. additionThe fractions containing the desired product
  7. customwere collected
  8. concentrationconcentrated