HRID1510220

反应详情

EQUATION

反应方程式

HRID 1510220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 2-anilino-N-[4-(4-pyridinyl)phenyl]acetamide (50.0 mg) and [(tert-butoxycarbonyl)amino]acetic acid (86.6 mg) in N,N-dimethylformamide (1.0 mL) were added diisopropylethylamine (0.189 mL) and N-[(dimethylamino) (3H-[1,2,3]triazolo[4,5-b]pyridin-3-yloxy)methylene]-N-methylmethanaminium hexafluorophosphate (207 mg) at ambient temperature and the mixture was stirred at the same temperature for 24 hours. Water (3.0 mL) was added to the mixture and the resulting mixture was extracted with ethyl acetate (6.0 mL). The organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by preparative thin-layer chromatography (10% methanol in chloroform) to afford tert-butyl{2-oxo-2-[(2-oxo-2-{[4-(4-pyridinyl)phenyl]amino}ethyl)(phenyl)amino]ethyl}carbamate (36.5 mg) as yellow crystals.

WORKUP

后处理

  1. extractionthe resulting mixture was extracted with ethyl acetate (6.0 mL)
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by preparative thin-layer chromatography (10% methanol in chloroform)