HRID631810

反应详情

EQUATION

反应方程式

HRID 631810 的结构方程式

PROCEDURE

实验过程

To 2-chloro-4-methyl-5-nitro-pyridine (250 mg, 1.45 mmol) was added potassium carbonate (320 mg, 2.32 mmol) followed by ethylenediamine (4.2 g, 70 mmol). The mixture turned hot and was filtered after cooling through kieselguhr. The filtrate was concentrated under reduced pressure and purified by column chromatography (silica, gradient of 1 to 10% methanol containing 7N ammonia in DCM) to yield 205 mg (1.04 mmol, 72%) MS(ESI) m/z=197.1 [M+1]+.

WORKUP

后处理

  1. filtrationwas filtered
  2. temperatureafter cooling through kieselguhr
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. custompurified by column chromatography (silica, gradient of 1 to 10% methanol containing 7N ammonia in DCM)
  5. customto yield 205 mg (1.04 mmol, 72%) MS(ESI) m/z=197.1 [M+1]+