HRID1817652
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
A solution of 4-[1-(1-cyclopentylbut-3-yn-1-yl)-1H-pyrazol-4-yl]-7-[2-(trimethylsilyl)-ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidine (52 mg, 0.12 mmol) in DCM (3 mL) and TFA (1 mL) was stirred for 2 hours. The solvents were removed in vacuo. The resulting residue was dissolved 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 product (30 mg, 60%).
WORKUP
后处理
- customThe solvents were removed in vacuo
- dissolutionThe resulting residue was dissolved in THF (3 mL)
- addition6N NaOH (2 mL) was added
- customthe mixture was 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)