反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was removed in vacuo
- dissolutionThe residue was dissolved in THF (2 mL)
- addition6 N NaOH (1 mL) was added
- stirringThe mixture was stirred at room temperature for 1 hour
- customwas partitioned between water and ethyl acetate
- dry with materialThe organic layer was dried over sodium sulfate
- customthe solvent was removed in vacuo
- customPurification via preparative-HPLC/MS (C18
- washeluting with a gradient of H2O and ACN containing 0.1% TFA)