HRID2387268

反应详情

EQUATION

反应方程式

HRID 2387268 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To propane-1-sulfonic acid (2,4-difluoro-3-formyl-phenyl)-amide (10, 102 mg, 0.32 mmol) in methanol (1.5 mL) was added 5-cyclopentyloxy-1H-pyrrolo[2,3-b]pyridine (P-0001, 65 mg, 0.32 mmol, prepared as described in Example 12) and potassium hydroxide (54 mg, 0.96 mmol) under an atmosphere of nitrogen. The reaction was stirred at room temperature for 3 hours. The reaction was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and filtrated. The filtrate was concentrated and purified by silica gel column chromatography eluting with 50% ethyl acetate in hexane to give a solid (11, 102 mg, 68%). MS (ESI) [M+H+]+=466.2.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltrated
  5. concentrationThe filtrate was concentrated
  6. custompurified by silica gel column chromatography
  7. washeluting with 50% ethyl acetate in hexane
  8. customto give a solid (11, 102 mg, 68%)