反应详情

12 g (43 mmol) of 8-(4-methoxyphenylamino)-caprylic acid methyl ester are dissolved in 400 cc. of ether. 5.1 g (50 mmol) of triethylamine are added thereto. 7.3 g (43 mmol) of 4-methoxybenzoic acid chloride are added dropwise to the mixture with stirring and cooling with ice. After the addition, stirring is continued at 25° C. for 5 hours. The separated triethylamine-hydrochloride is filtered off with suction and the ethereal phase is washed in sequence with water, 5% bicarbonate solution, water, 2 n hydrochloric acid and water is dried over Na2SO4, and the solvent is distilled off. The crude product is used in the next step without any further purification.

1. temperaturecooling with ice
2. additionAfter the addition
3. stirringstirring
4. filtrationThe separated triethylamine-hydrochloride is filtered off with suction
5. washthe ethereal phase is washed in sequence with water, 5% bicarbonate solution, water, 2 n hydrochloric acid and water
6. dry with materialis dried over Na2SO4
7. distillationthe solvent is distilled off
8. customThe crude product is used in the next step without any further purification