HRID1501506

反应详情

EQUATION

反应方程式

HRID 1501506 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[1-(1-Cyclopentylbut-3-en-1-yl)-1H-pyrazol-4-yl]-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidine (13 mg, 0.030 mmol) was dissolved in DCM (3 mL) and TFA (0.5 mL) was added. The resulting solution was stirred at room temperature for 3 hours. The solvent was removed in vacuo. The residue was dissolved in THF (2 mL), and 6 N NaOH (1 mL) was added. The mixture was stirred at room temperature for 1 hour, and then 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 product (10 mg, 80%).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in THF (2 mL)
  3. addition6 N NaOH (1 mL) was added
  4. stirringThe mixture was stirred at room temperature for 1 hour
  5. customwas partitioned between water and ethyl acetate
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. customthe solvent was removed in vacuo
  8. customPurification via preparative-HPLC/MS (C18
  9. washeluting with a gradient of H2O and ACN containing 0.1% TFA)