反应详情

A mixture of 15.8 g (0.039 mole) of 3,6-bis(4-chlorobutyryl)-N-ethylcarbazole, prepared from N-ethylcarbazole and 4-chlorobutyryl chloride, 75 ml of 40% aqueous dimethylamine and 2 g of potassium iodide in 175 ml of p-dioxane is heated in a reaction bomb with stirring for 44 hours. The reaction mixture is concentrated to one-half its original volume in vacuo and diluted with 500 ml of water. The semi-solid which separates is dissolved in ether and washed repeatedly with water and dried over magnesium sulfate to give the free base which is treated with fumaric acid and recrystallized from butanone to give 3,6-bis(4-dimethylaminobutyryl)-N-ethylcarbazole bis acid fumarate. M.P. 94°-98°C.

1. temperatureis heated in a reaction bomb
2. concentrationThe reaction mixture is concentrated to one-half its original volume in vacuo
3. additiondiluted with 500 ml of water
4. dissolutionThe semi-solid which separates is dissolved in ether
5. washwashed repeatedly with water
6. dry with materialdried over magnesium sulfate
7. customto give the free base which
8. customrecrystallized from butanone