HRID45041

反应详情

EQUATION

反应方程式

HRID 45041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-[1-(1-cyclopentyl-4,4-difluorobut-3-en-1-yl)-1H-pyrazol-4-yl]-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidine (41 mg, 0.086 mmol) in DCM (3 mL) and TFA (1.5 mL) was stirred for two hours at room temperature. The solution was then concentrated in vacuo. The resulting residue was redissolved in THF (3 mL), and 6N NaOH (2 mL) was added. After stirring for 1 hour, the mixture was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was removed in vacuo. Purification via preparative-HPLC/MS (C18 eluting with a gradient of H2O and ACN containing 0.1% TFA) afforded the desired product (39 mg, 98%).

WORKUP

后处理

  1. concentrationThe solution was then concentrated in vacuo
  2. dissolutionThe resulting residue was redissolved in THF (3 mL)
  3. addition6N NaOH (2 mL) was added
  4. customthe mixture was partitioned between water and ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was removed in vacuo
  7. customPurification via preparative-HPLC/MS (C18
  8. washeluting with a gradient of H2O and ACN containing 0.1% TFA)