反应详情

温度

90 °C

To a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser, dropping funnel and a nitrogen atmosphere are charged 16.2 g (30 mmol) of the product of Example 62, 3.7 g (66 mmol) of powdered potassium hydroxide and 100 mL of 2-ethoxyethanol. To the resulting red solution are then added 10.9 g (66 mmol) of 1-bromohexane are added dropwise over 30 minutes. The mixture is heated to 90° C. for 20 hours and filtered hot. The filtrate is warmed to 100° C. and 1 mL of acetic acid is added. The solution is cooled to 0° C. to give a precipitate. The crude yellow product is recrystallized from 70 mL of 2-ethoxyethanol to give the title compound in a yield of 13.1 g as a yellow solid melting at 118°-121° C.

1. customTo a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser
2. additionare added dropwise over 30 minutes
3. filtrationfiltered hot
4. temperatureThe filtrate is warmed to 100° C.
5. addition1 mL of acetic acid is added
6. temperatureThe solution is cooled to 0° C.
7. customto give a precipitate
8. customThe crude yellow product is recrystallized from 70 mL of 2-ethoxyethanol