HRID1850693

反应详情

EQUATION

反应方程式

HRID 1850693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-cyano-N-(2-methyl-3-phenyl-imidazol-4-yl)acetamide (100 mg, 0.4162 mmol) in Ethanol (1.5 mL) was sequentially added sodium acetate (68.28 mg, 0.8324 mmol), 2,2,2-trichloroacetonitrile (0.051 mL, 0.5016 mmol) and the reaction was stirred at room temperature for 4 h. A further 10 mg of sodium acetate and 10 uL 2,2,2-trichloroacetonitrile was sequentially added and the mixture was stirred for a further 2 h at RT. The reaction was concentrated in vacuo and the residue was partitioned between water and EtOAc. Combined organic extract was washed with brine, dried (MgSO4) and concentrated in vacuo to give 3-amino-4,4,4-trichloro-2-cyano-N-(2-methyl-1-phenyl-1H-imidazol-5-yl)but-2-enamide as a redish oil. (153 mg, 79%). MS (ES+) 384.0.

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 2 h at RT
  2. concentrationThe reaction was concentrated in vacuo
  3. customthe residue was partitioned between water and EtOAc
  4. extractionCombined organic extract
  5. washwas washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo