HRID1662278

反应详情

EQUATION

反应方程式

HRID 1662278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a mixture of 2,6-dimethylnitrobenzene (151 g, 1.0 mol), acetic acid (1200 ml), and conc. H2SO4 (60 ml) was added iodine (102 g, 0.4 mol) and periodic acid dehydrate (205 g, 0.9 mol). The resulting solution was heated at 90° C. for 4 days. After cooling to room temperature, the reaction mixture was diluted with water (2000 ml). The yellow crystals were filtered and washed with water to give 220 g of pure product (79%). 1H-NMR δ (DMSO-d6, 300 MHz): 7.95 (d, J=7.8 Hz, 1H), 7.08 (d, J=7.8 Hz, 1H), 2.27 (s, 3H), 2.16 (s, 3H).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationThe yellow crystals were filtered
  3. washwashed with water