HRID383568

反应详情

EQUATION

反应方程式

HRID 383568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 1-(2,4-difluorophenyl)-N-ethyl-1H-pyrazol-5-amine (1.15 g, 5.16 mmol) in 4.0 mL of EtOAc, 2.0 mL of EtOH and 4.0 mL of 5-6 N HCl in 2-propanol was cooled in an ice/brine bath and treated with isoamyl nitrite (0.70 mL, 5.28 mmol) drop wise. After stirring at this temperature for 15 min, the reaction was quenched by the addition of 28-30% NH4OH solution and EtOAc, forming a deep blue solution. The EtOAc layer was separated, washed with brine, dried and concentrated to afford the title compound as a brown crystalline solid. MS (ES+): 253.1 (M+H)+.

WORKUP

后处理

  1. customthe reaction was quenched by the addition of 28-30% NH4OH solution and EtOAc
  2. customforming a deep blue solution
  3. customThe EtOAc layer was separated
  4. washwashed with brine
  5. customdried
  6. concentrationconcentrated