Реакция #524675

Уравнение реакции

3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid

methanol

→

methyl 3-(2-chloro-4-trifluoromethylphenoxy)benzoate

Выход 98.0%

Условия реакции

Обработка

1. 1
   ДругоеTo a 300 ml, 3-necked flask equipped with a stirrer
2. 2
   Другоеgas bubbling tube, condenser
3. 3
   Другоеthermometer and drying tube
4. 4
   ДругоеAnhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm)
5. 5
   Другоеrises to 50° C
6. 6
   Температураwith external heating for 4 hours
7. 7
   Температураcooled
8. 8
   Другоеthe solvent removed in vacuo
9. 9
   workup.DISSOLUTIONthe residue dissolved in CCl4 (200 ml)
10. 10
    Другоеtriturated with water (50 ml)
11. 11
    ДругоеThe decanted
12. 12
    Сушкаdried (anh. MgSO4) CCl4 layer
13. 13
    Другоеto give 12.2 g

Методика

To a 300 ml, 3-necked flask equipped with a stirrer, gas bubbling tube, condenser, thermometer and drying tube is charged anhydrous methanol (100 ml) and 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid (12 g., 0.038 mole). Anhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm) rises to 50° C. The reaction mixture is then maintained at 50° C. with external heating for 4 hours, then cooled, the solvent removed in vacuo and the residue dissolved in CCl4 (200 ml) and triturated with water (50 ml). The decanted and dried (anh. MgSO4) CCl4 layer is reduced in vacuo to give 12.2 g. of methyl 3-(2-chloro-4-trifluoromethylphenoxy)benzoate (98% yield).

Источник