HRID581072

反应详情

EQUATION

反应方程式

HRID 581072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.1 g (0.75 mmol) of hydroxybenzotriazole (HOBt) and 0.14 g (0.75 mmol) of 1-(3dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) are introduced at 0° C. into a reaction mixture comprising 0.15 g (0.68 mmol) of the acid obtained in Step F dissolved in 3 ml of anhydrous DMF. After the addition of 1.02 mmol of a 10% solution of methylamine in benzene, stirring is maintained for 24 hours and then the solvent is evaporated off in vacuo. The residue obtained is taken up in dichloromethane and then washed with water. The organic phase is dried over magnesium sulphate and then concentrated in vacuo. Chromatography over silica gel (eluant:AcOEt/PE:70/30) allows isolation of the title amide in the form of a clear oil.

WORKUP

后处理

  1. temperatureis maintained for 24 hours
  2. customthe solvent is evaporated off in vacuo
  3. customThe residue obtained
  4. washwashed with water
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. concentrationconcentrated in vacuo