HRID1354722

反应详情

EQUATION

反应方程式

HRID 1354722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.095 g of HATU, 0.068 g of HOBT and 0.035 ml of triethylamine were added to a solution of 0.047 g of 2′,4′-difluorobiphenyl-4-carboxylic acid and 0.058 g of N-[1-(4-aminophenyl)pyrrolidin-3-yl]-N-methylacetamide in 2 ml of DMF at 0° C. After 10 minutes, the solution was allowed to reach room temperature and was stirred at this temperature overnight. The solvent was then removed in vacuo, and the residue was taken up in water/ethyl acetate. The ethyl acetate phase was washed with 10% NaHCO3 solution and water. The ethyl acetate phase was dried over sodium sulfate, and the solvent was removed in vacuo. The residue was purified by preparative HPLC. The desired product was obtained. Molecular weight 449.19 (C26H25F2N3O2), MS: 450 (M+H+).

WORKUP

后处理

  1. customto reach room temperature
  2. customThe solvent was then removed in vacuo
  3. washThe ethyl acetate phase was washed with 10% NaHCO3 solution and water
  4. dry with materialThe ethyl acetate phase was dried over sodium sulfate
  5. customthe solvent was removed in vacuo
  6. customThe residue was purified by preparative HPLC