HRID2354618

反应详情

EQUATION

反应方程式

HRID 2354618 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

The mixture of 3′-Amino-4′-benzoyl-6-methyl-biphenyl-3-carboxylic acid cyclopropylamide from Example 15 (20 mg, 0.054 mmol) and formamide (2.9 mg, 0.065 mmol) in 0.7 mL acetic acid was stirred at 180° C. for 10 minutes in microwave. The solvents were removed under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate and was washed with sat. aqueous NaHCO3 (10 mL), water (10 mL), and brine (10 mL), dried over MgSO4, and the solvents were evaporated. The residue was purified by preparative TLC sheet (methylene chloride:methanol=10:1) to give a colorless solid (4.6 mg, 22%)

WORKUP

后处理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionThe residue was dissolved in 50 mL of ethyl acetate
  3. washwas washed with sat. aqueous NaHCO3 (10 mL), water (10 mL), and brine (10 mL)
  4. dry with materialdried over MgSO4
  5. customthe solvents were evaporated
  6. customThe residue was purified by preparative TLC sheet (methylene chloride:methanol=10:1)