HRID63247

反应详情

EQUATION

反应方程式

HRID 63247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Benzoylacetonitrile (500 mg, 3.44 mmol) and o-tolylhydrazine hydrochloride (574 mg, 3.61 mmol) were placed in a microwave vial and dissolved in methanol (1.7 mL). The reaction vessel was sealed, placed in a microwave oven and heated at 120° C. for 1 hour. After this period, the reaction mixture was concentrated onto silica gel and purified by flash chromatography (0-50% ethyl acetate/hexanes gradient) to afford the desired intermediate, 5-phenyl-2-o-tolyl-2H-pyrazol-3-ylamine (392 mg). LC/MS: Calc. C16H15N3 249.13 amu; Obs. [M+H]+=250.2 amu.

WORKUP

后处理

  1. customThe reaction vessel was sealed
  2. customplaced in a microwave oven
  3. waitAfter this period
  4. concentrationthe reaction mixture was concentrated onto silica gel
  5. custompurified by flash chromatography (0-50% ethyl acetate/hexanes gradient)