反応 #55537

反応方程式

1,3-diaminopropane

2-nitro-2'-hydroxy-5'-methyl-azobenzene

water

→

2-(2'-hydroxy-5'-methylphenyl)-benzotriazole

溶媒

xylene

反応条件

後処理

1. 1
   温度the whole is heated, with the exclusion of air
2. 2
   workup.ADDITIONis then added
3. 3
   その他The aqueous phase is separated
4. 4
   抽出the organic phase is extracted with aqueous hydrochloric acid
5. 5
   洗浄washed with water until neutral
6. 6
   workup.DISTILLATIONThe xylene is distilled off
7. 7
   その他to leave 7.7 g of crude product

実験手順

11.6 g of 1,3-diaminopropane (0.16 mol) and 2 g of copper-II-acetate (0.01 mol) are placed into 50 ml of water and the whole is heated, with the exclusion of air and with stirring, to 85°-90° C. A solution of 10 g of 2-nitro-2'-hydroxy-5'-methyl-azobenzene (0.04 mol) in 100 ml of xylene heated to 60° C. is then added, and after 20 hours the reaction mixture is cooled to room temperature. The aqueous phase is separated, and the organic phase is extracted with aqueous hydrochloric acid, and then washed with water until neutral. The xylene is distilled off to leave 7.7 g of crude product. Analysis of the crude product by means of LC (liquid chromatography) gives 86% of theory of 2-(2'-hydroxy-5'-methylphenyl)-benzotriazole.

出典