HRID243107

反应详情

EQUATION

反应方程式

HRID 243107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2,6-difluoro-3-nitrobenzoic acid (1.0 g, 4.92 mmol) in IMS (5 mL) and water (5 mL) were added Et3N (1.23 mL, 8.86 mmol) and cyclopropylamine (360 μL, 5.17 mmol). The reaction mixture was stirred at RT for 28 h. The pH of the solution was adjusted to 1 by addition of 1M aqueous HCl. A precipitate formed and this solid was collected by filtration, washing with water to afford the title compound (841 mg, 71%) as a yellow solid. 1H NMR (CDCl3, 400 MHz): δ 8.78 (1H, s), 8.28 (1H, dd, J=9.45, 5.85 Hz), 6.49 (1H, m), 2.84 (1H, m), 0.85 (2H, m), 0.68 (2H, m)

WORKUP

后处理

  1. customA precipitate formed
  2. filtrationthis solid was collected by filtration
  3. washwashing with water