HRID2097623

反应详情

EQUATION

反应方程式

HRID 2097623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(3-Cyanophenyl)-4-methyl-1,2,5-oxadiazole-3-carboxamide (25 mg, 0.11 mmol) was suspended in benzene (2 mL) under an atmosphere of nitrogen. Phosphorus pentachloride (25 mg, 0.12 mmol) was added and the solution was heated at reflux for 2.5 hrs. The reaction was then evaporated to dryness. The crude was dissolved in EtOH (1.6 mL) and hydroxylamine (200 μL, 3 mmol, 50% solution in water) was added to the reaction. The crude was purified by preparative LCMS to afford the desired product (2.9 mg). MF═C11H9N5O2; LCMS calculated for C11H9N5O2 (M+H)+: m/z=244.1.

WORKUP

后处理

  1. temperaturethe solution was heated
  2. temperatureat reflux for 2.5 hrs
  3. customThe reaction was then evaporated to dryness
  4. dissolutionThe crude was dissolved in EtOH (1.6 mL)
  5. customThe crude was purified by preparative LCMS