HRID1581743

反应详情

EQUATION

反应方程式

HRID 1581743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe resulting mixture was filtered
  2. concentrationconcentrated in vacuo to a pale yellow oil
  3. dissolutionThis was dissolved in DCM (5 mL)
  4. washwashed with NaHCO3 (2 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated