HRID425305

反应详情

EQUATION

反应方程式

HRID 425305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dichloroacetic acid (0.35 mL, 4.2 mmol) was added to a mixture of compound 6 (1.04 g, 2.1 mmol), benzyltriethyl ammonium bromide (1.65 g, 6.1 mmol) and sodium nitrite (2.9 g, 42.1 mmol) in dibromomethane (44 mL). The mixture was stirred at room temperature for 18 hours in the dark. The reaction mixture was then concentrated tad the resulting residue was purified by column chromatography (95% dichloromethane/5% methanol) to afford 393 mg 34% yield of 4-(2-(5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-ylthio)acetamido)-3-chlorobenzoic acid (7).

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated tad the resulting residue
  2. customwas purified by column chromatography (95% dichloromethane/5% methanol)