反应详情

温度

110 °C

To a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser, dropping funnel and a nitrogen atmosphere are charged 26.3 g (70 mmol) of the product of Example 54, 10.6 g (77 mmol) of potassium carbonate, 50 mg of potassium iodide, and 50 mL of 2-ethoxyethanol. The suspension is warmed to 110° C., and 10.8 g (77 mmol) of 1-bromohexane are added dropwise over 30 minutes. After 8 hours, the reaction mixture is cooled to room temperature, the precipitate is removed by filtration, washed with water to pH 6, rinsed with methanol and dried at 70° C. under vacuum. The crude beige product (26.9 g) is recrystallized twice from 600 mL of 2-ethoxyethanol to give the title compound in a yield of 18.6 g as a yellow solid melting at 147°-149° C., purity 98.7% (DSC assay).

1. customTo a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser
2. temperaturethe reaction mixture is cooled to room temperature
3. customthe precipitate is removed by filtration
4. washwashed with water to pH 6
5. washrinsed with methanol
6. customdried at 70° C. under vacuum
7. customThe crude beige product (26.9 g) is recrystallized twice from 600 mL of 2-ethoxyethanol