反应详情

温度

45 °C

4-toluenesulfonyl chloride (162 g), toluene (363.3 g) and 2-(2-Thienyl)ethanol (104 g) are combined. Triethylamine (93 g) is added maintaining the temperature lower than 45° C. After 4 hrs, the mixture is washed with aqueous phosphoric acid, aqueous sodium hydroxide and then water. The organic phase is distilled off under vacuum. Isopropanol (314 g) and heptanes (365.9 g) are added. The batch is crystallized by cooling and isolated at −15° C. The crystals are filtered and washed with heptanes (175 mL). The crystals are then dried under vacuum at room temperature until a melting point of 30° C. is obtained.

1. washthe mixture is washed with aqueous phosphoric acid, aqueous sodium hydroxide
2. distillationThe organic phase is distilled off under vacuum
3. additionIsopropanol (314 g) and heptanes (365.9 g) are added
4. customThe batch is crystallized
5. temperatureby cooling
6. customisolated at −15° C
7. filtrationThe crystals are filtered
8. washwashed with heptanes (175 mL)
9. customThe crystals are then dried under vacuum at room temperature until a melting point of 30° C.
10. customis obtained