反应详情

温度

70 °C

A suspension of 0.840 g of 2-chloro-4-nitro-1-nitrosobenzene in 20 ml of glacial acetic acid was heated to 70° C. and treated while stirring with a solution, heated to 110° C., of 0.926 g of 4-amino-4'-hydroxybiphenyl [prepared according to Chem. Berichte 27 (1894) 2627] in 43 ml of glacial acetic acid. The dark solution was stirred at 70° C. for a further 2.25 hours, then cooled to room temperature and extracted with methylene chloride. The extracts were washed with water, 10% sodium hydrogen carbonate solution and again with water, dried over sodium sulphate and concentrated in vacuo. Thus yielding 1.3 g of crude 2-chloro-4-nitro-4'-(4-hydroxyphenyl)azobenzene as brown crystals.

1. additiontreated
2. stirringThe dark solution was stirred at 70° C. for a further 2.25 hours
3. temperaturecooled to room temperature
4. extractionextracted with methylene chloride
5. washThe extracts were washed with water, 10% sodium hydrogen carbonate solution and again with water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated in vacuo