HRID1581743
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
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
To a solution of 4-{6-ethoxy-5-[3-ethyl-4,5,6,7-tetrahydro-7-oxo-2-(2-pyridylmethyl)-2H-pyrazolo[4,3-d]pyrimidin-5-yl]-3-pyridinylsulfonyl}-1-ethylpiperazine (50 mg, 0.09 mmol, from step (b) above) in toluene (1 mL), was added 10% Pd/C (25 mg, 50% w/w) and trifluoroacetic acid (14 μL). The mixture was heated to 200° C. under nitrogen at 34.5 kPa (5 psi) for 6 hours. The resulting mixture was filtered and concentrated in vacuo to a pale yellow oil. This was dissolved in DCM (5 mL) and washed with NaHCO3 (2 mL), dried over MgSO4 and concentrated to give a brown oil (42 mg, 84%) as product.
WORKUP
后处理
- filtrationThe resulting mixture was filtered
- concentrationconcentrated in vacuo to a pale yellow oil
- dissolutionThis was dissolved in DCM (5 mL)
- washwashed with NaHCO3 (2 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated