HRID1599083

反应详情

EQUATION

反应方程式

HRID 1599083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of N-(1,3,5-Trimethyl-1H-pyrazol-4-yl)-benzene-1,2-diamine (7.56 g, 35.0 mmol) and 2-bromo-N-isopropyl-N-(4-methoxy-phenyl)-acetamide (7.18 g, 38.5 mmol) in DMF (70 mL) was added potassium carbonate (14.5 g, 105 mmol) and potassium iodide (581 mg, 3.5 mmol). The solution was heated at 80° C. for 15 h and subsequently poured into DCM (100 mL). The mixture was extracted with H2O (×4), 1N HCl (×2) and brine, dried over MgSO4 and concentrated in vacuo. The resulting foam was purified by trituration with Et2O to yield the title compound (11.9 g):

WORKUP

后处理

  1. extractionThe mixture was extracted with H2O (×4), 1N HCl (×2) and brine
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe resulting foam was purified by trituration with Et2O