Method for synthesizing 2-chlorine-4-trifluoromethyl phenol
A technology of trifluoromethylphenol and trifluoromethyl, which is applied in the field of herbicide preparation, can solve the problems of high production cost, long reaction time, and unsuitable use of trifluoromethylphenol, and achieve convenient post-processing and short reaction time , the effect of increasing the yield
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Embodiment 1
[0014] Into a round bottom flask was added 4-(trifluoromethyl)benzaldehyde (6.75 mmol, 1.0 equiv), CH 2 Cl 2 (20 mL), then add mCPBA (6.78 mmol, 1.0 equiv), stir at room temperature for 2 h, add 15 ml saturated NaHSO 3 The aqueous solution was transferred to a separatory funnel for extraction, the organic phases were collected and combined, dried and filtered with anhydrous sodium sulfate to obtain a 4-(trifluoromethyl)phenol solution, and the monitored yield was 85%. Under inert gas conditions, add NCS (5.74 mmol) and CH in a round bottom flask 2 Cl 2 (20.0 mL), cooled to -78 °C, added ZrCl 4 (0.115 mmol), followed by adding 4-(trifluoromethyl)phenol solution, the reaction was stirred at room temperature for 6 hours, after the reaction was completed, saturated NaHCO 3 The aqueous solution was extracted, the organic phases were collected and combined, and the solvent was removed to obtain 2-chloro-4-trifluoromethylphenol with a yield of 88%.
Embodiment 2
[0016] Add 4-(trifluoromethyl)benzaldehyde (6.75 mmol, 1.0 equiv) to a round bottom flask, CH 2 Cl 2 (20 mL), then add mCPBA (0.68 mmol, 0.1 equiv), stir at room temperature for 2 h, add 15 ml saturated NaHSO 3 The aqueous solution was transferred to a separatory funnel for extraction, the organic phases were collected and combined, dried and filtered with anhydrous sodium sulfate to obtain a 4-(trifluoromethyl)phenol solution, and the monitored yield was 44%. Under inert gas conditions, add NCS (2.97 mmol) and CH in a round bottom flask 2 Cl 2 (20.0 mL), cooled to -78 °C, added ZrCl 4 (0.06 mmol), followed by adding 4-(trifluoromethyl)phenol solution, the reaction was stirred at room temperature for 6 hours, after the reaction was completed, saturated NaHCO 3 The aqueous solution was extracted, the organic phases were collected and combined, and the solvent was removed to obtain 2-chloro-4-trifluoromethylphenol with a yield of 88%.
Embodiment 3
[0018] Into a round bottom flask was added 4-(trifluoromethyl)benzaldehyde (6.75 mmol, 1.0 equiv), CH 2 Cl 2 (40 mL), then add mCPBA (67.8 mmol, 10 equiv), stir at room temperature for 2 h, add 30 ml saturated NaHSO 3 The aqueous solution was transferred to a separatory funnel for extraction, the organic phases were collected and combined, dried and filtered with anhydrous sodium sulfate to obtain a 4-(trifluoromethyl)phenol solution, and the monitored yield was 86%. Under inert gas conditions, add NCS (2.9 mmol, ) and CH in a round bottom flask 2 Cl 2 (20.0 mL), cooled to -78 °C, added ZrCl 4 (0.116 mmol), then added 4-(trifluoromethyl)phenol solution, the reaction was stirred at room temperature for 6 hours, after the reaction was completed, saturated NaHCO 3 The aqueous solution was extracted, the organic phases were collected and combined, and the solvent was removed to obtain 2-chloro-4-trifluoromethylphenol with a yield of 70%.
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