HRID1593529

反应详情

EQUATION

反应方程式

HRID 1593529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To 46 mg 1-[6-(2-Chloro-4-methoxy-5-methyl-phenyl)-5-methyl-pyrazin-2-yl]-1H-benzotriazole (0.12 mmol) in 200 μL toluene was added 100 μL 0.5 M 2,5-dimethoxyphenyl magnesium bromide in THF. The solution is subjected three times to 3 GHz microwave radiation heating to 150° C. for 15 min. After quenching with saturated ammonium chloride, the organic phase was directly subjected to column chromatography eluting with hexanes DCM followed by hexane ethyl acetate (0.1% Et3N) . Fractions containing the desired product were pooled and concentrated to give a residue that was further purified by RP—HPLC eluting with acetonitrile water (0.03% TFA) giving 2.6 mg of the title compound.

WORKUP

后处理

  1. customAfter quenching with saturated ammonium chloride
  2. washeluting with hexanes DCM
  3. additionFractions containing the desired product
  4. concentrationconcentrated
  5. customto give a residue that
  6. customwas further purified by RP—HPLC
  7. washeluting with acetonitrile water (0.03% TFA)