HRID1259323

反应详情

EQUATION

反应方程式

HRID 1259323 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Fluorobenzonitrile (7.0 g, 58 mmol) and 2-methylpropane-1,2-diamine (14 g, 160 mmol) were heated in a sealed vial in a microwave reactor (Biotage) at 180° C. for 25 minutes in two batches. Each batch was dissolved in methanol (50 mL) and then concentrated with silica to dryness. Flash chromatography on silica of each batch with neat acetonitrile and 2% triethylamine in acetonitrile as eluents gave 4-(2-amino-2-methylpropylamino)benzonitrile (9.58 g, 88% combined yield) as a white solid.

WORKUP

后处理

  1. concentrationconcentrated with silica to dryness