HRID2382766

反应详情

EQUATION

反应方程式

HRID 2382766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5-chloro[1,2,4]triazolo[1,5-a]pyridin-2-amine ((A4), 10.0 g; 59.32 mmol; 1.0 eq.) in cyclohexylamine (60 mL) was heated to reflux for 52 h. Reaction mixture was taken up in MTBE and filtered. The resulting cake was washed with MTBE and filtrate was concentrated to dryness. Residue was purified by flash chromatography (Hept/EtOAc, 1:1) to give the title compound as a beige powder (8.08 g, 59%). HPLC, Rt: 2.46 min. (purity 98.9%). LC/MS, M+(ESI): 231.9.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 52 h
  3. customReaction mixture
  4. filtrationfiltered
  5. washThe resulting cake was washed with MTBE and filtrate
  6. concentrationwas concentrated to dryness
  7. customResidue was purified by flash chromatography (Hept/EtOAc, 1:1)