HRID1057487

反应详情

EQUATION

反应方程式

HRID 1057487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[(phenylmethoxy)carbonylamino]butanoic acid (1.1 eq) was dissolved in methylene chloride (0.2M) followed by the addition of 1-[3-(Dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (EDCA) (1.2 eq) and triethylamine (1.5 eq). The mixture was stirred at room temperature under nitrogen for 30 mins, followed by addition of 2,3-diaminopyridine. The mixture was then stirred at room temperature for 48 hrs., quenched with saturated sodium carbonate and extracted with ether. The organic phase was concentrated in vacuo and chromatographed on silica gel. (10% MeOH/CH2Cl2). EI-MS m/z 329 (M+H)+.

WORKUP

后处理

  1. stirringThe mixture was then stirred at room temperature for 48 hrs
  2. custom, quenched with saturated sodium carbonate
  3. extractionextracted with ether
  4. concentrationThe organic phase was concentrated in vacuo
  5. customchromatographed on silica gel