反応 #1973972

反応方程式

iodine

2-bromo-6-tert-butylaniline

sodium bicarbonate

sodium thiosulfate

→

oil

収率 65.0%

2-bromo-6-tert-butyl-4-iodoaniline

収率 65.0%

溶媒

water

反応条件

後処理

1. 1
   温度The mixture was cooled in an ice bath
2. 2
   抽出extracted by ethyl acetate
3. 3
   乾燥dried with sodium sulfate
4. 4
   ろ過filtered
5. 5
   その他evaporated
6. 6
   その他The residue was purified on silica gel eluting with 5% ethyl acetate in hexane

実験手順

In a 50 mL round-bottom flask was added 2-bromo-6-tert-butylaniline [prepared by the method of Onitsuka, et. al. Organometallics, 25(5), 2006, pp 1270-1278] (1.18 g, 5.17 mmol) and sodium bicarbonate (0.782 g, 9.31 mmol) in water (5 ml). The mixture was cooled in an ice bath and iodine (1.444 g, 5.69 mmol) was added in several portions. The mixture was warmed to ambient temperature and stirred for 16 h. The mixture was treated with aqueous sodium thiosulfate, extracted by ethyl acetate, dried with sodium sulfate, filtered and evaporated. The residue was purified on silica gel eluting with 5% ethyl acetate in hexane to give an oil (1.2 g, 65%).

出典