HRID555984

反应详情

EQUATION

反应方程式

HRID 555984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of N-(6-bromo-imidazo[1,2-a]pyridin-2-yl)-2,2,2-trifluoro-acetamide (9.0 g, 29.2 mmol) in DME (90 ml) and 1.27 M aqueous potassium phosphate (80.5 ml, 102.3 mmol) is heated at 90° C. overnight. After cooling to room temperature, the two layers are separate and the aqueous portion is extracted with EtOAc. The combined organic extracts are concentrated in vacuo to afford a brown oil. Iso-hexanes is added to the oil resulting in the formation of a solid. The excess iso-hexanes is decanted off and the remaining DME is azeotroped with THF (2×50 ml) to afford the title compound as a solid [MH+ 211.93].

WORKUP

后处理

  1. customthe two layers are separate
  2. extractionthe aqueous portion is extracted with EtOAc
  3. concentrationThe combined organic extracts are concentrated in vacuo
  4. customto afford a brown oil
  5. customresulting in the formation of a solid
  6. customThe excess iso-hexanes is decanted off
  7. customthe remaining DME is azeotroped with THF (2×50 ml)