HRID2382773

反应详情

EQUATION

反应方程式

HRID 2382773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of 5-chloro-7-(trifluoromethyl)[1,2,4]triazolo[1,5-a]pyridin-2-amine ((A7), 183.00 mg; 0.77 mmol; 1.00 eq.) and isopropylamine (664.58 μl; 7.74 mmol; 10.00 eq.) in n-butanol (1.50 mL) was heated at 120° C. for 1 h30 under MW irradiation. The reaction mixture was then concentrated under vacuum till dryness. The solid obtained was triturated in water/MTBE and filtered. The solid which precipitated in mother liquor was finally filtered, washed with water and dried under vacuum at 40° C. to give the title compound as an off-white solid (122 mg, 61%). HPLC, Rt: 2.64 min. (purity 86.5%). LC/MS, M+(ESI): 259.9, M−(ESI): 257.9.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated under vacuum till dryness
  2. customThe solid obtained
  3. customwas triturated in water/MTBE
  4. filtrationfiltered
  5. customThe solid which precipitated in mother liquor
  6. filtrationwas finally filtered
  7. washwashed with water
  8. customdried under vacuum at 40° C.