HRID884816

反应详情

EQUATION

反应方程式

HRID 884816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a stirred solution of 3-[5-amino-4-(3-hydroxy-benzoyl)-pyrazol-1-yl]-N-cyclopropyl-4-methylbenzamide (75 mg, 0.2 mmol) and 4-chloromethyl-2,2-dimethyl-[1,3]dioxolane (36 mg, 0.24 mmol) were dissolved in DMF (4 ml) was added K2CO3 and the mixture stirred at 150° C. for 2 h in microwave oven. The solvent was removed, residue was dissolved in EtOAc, washed by water, brine, dried over Na2SO4, and concentrated. The residue was purified by column chromatography (EtOAc: Hex=3:1) and the product was obtained as a colorless oil (18 mg, 18%). HPLC (4 minute gradient) tR 2.57 min; MS m/z 491.11 [M+H]+.

WORKUP

后处理

  1. customThe solvent was removed
  2. dissolutionresidue was dissolved in EtOAc
  3. washwashed by water, brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography (EtOAc: Hex=3:1)