反应详情

To a solution of 4-amino-3-iodo-5-nitrotoluene (14.0 g) in ethanol (70 ml) was added concentrated sulphuric acid (8 ml) dropwise, then the solution was heated to reflux and solid sodium nitrite (8.9 g) added in small amounts over 30 minutes. The mixture was refluxed a further one hour, and then was poured into ice water. The precipitate was washed with water and dried to yield 3-iodo-5-nitrotoluene (10.2 g). δ (360 MHz, DMSO-d6) 2.40 (3H, s, CH3), 8.07 (2H, bs, 2-H and 6-H) and 8.30 (1H, s, 4-H).

1. temperaturethe solution was heated
2. temperatureto reflux
3. temperatureThe mixture was refluxed a further one hour
4. washThe precipitate was washed with water
5. customdried