HRID1159978

反应详情

EQUATION

反应方程式

HRID 1159978 的结构方程式

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

The title compound was synthesized by combining N-{3-[3-(2-chloro-4-pyrimidinyl)pyrazolo[1,5-a]pyridin-2-yl]phenyl}-2,6-difluorobenzamide (200 mg, 0.43 mmol) (prepared according to a procedure similar to that described in Example 27, Step C), N-(5-amino-2,3-dihydro-1H-inden-2-yl)-2,2,2-trifluoroacetamide (127 mg, 0.52 mmol), hydrochloric acid (0.043 mmol, 43 μL 1M HCl/diethylether) and 2 mL isopropanol in a sealed vessel. The vial and contents were heated in a microwave synthesizer at 180° C. for 30 min. The reaction was cooled and concentrated. The residue was partitioned between EtOAc and saturated NaHCO3. The organic was washed with brine, dried with MgSO4 and concentrated. The crude material was purified by silica gel column chromatography (0-100% gradient; (90% DCM:9% MeOH:1% NH4OH/DCM)). Purification provided 278 mg (95%) of the coupled adduct. ESIMS (M+H)+=684.20.

WORKUP

后处理

  1. customprepared
  2. temperatureThe reaction was cooled
  3. concentrationconcentrated
  4. customThe residue was partitioned between EtOAc and saturated NaHCO3
  5. washThe organic was washed with brine
  6. dry with materialdried with MgSO4
  7. concentrationconcentrated
  8. customThe crude material was purified by silica gel column chromatography (0-100% gradient; (90% DCM:9% MeOH:1% NH4OH/DCM))
  9. customPurification