4-Hydroxy-3-nitrobenzotrifluoride synthesis
- Product Name:4-Hydroxy-3-nitrobenzotrifluoride
- CAS Number:400-99-7
- Molecular formula:C7H4F3NO3
- Molecular Weight:207.11
139-07-1
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400-99-7
Example 1: 400 mL of methanol, 20 g of dodecyldimethylbenzylammonium chloride and 180 g of 4-chloro-3-nitrobenzotrifluoride were added to a reaction flask with stirring turned on. Subsequently, 400 g of 50% sodium hydroxide solution was slowly added dropwise, with the dropwise acceleration controlled to raise the reaction temperature to 70°C in about 20 minutes. The reaction mixture was continued stirring at 65°C for 4 hours. Upon completion of the reaction, the mixture was cooled in an ice water bath and the pH was adjusted with concentrated hydrochloric acid to 3. 2-Nitro-4-trifluoromethylphenol was isolated by steam distillation, and about 50 mL of concentrated hydrochloric acid was added to the receiver to facilitate phase separation. After gas chromatographic analysis, 156 g of 2-nitro-4-trifluoromethylphenol was obtained with a purity of >98.5% and a yield of 91% of the theoretical value. The boiling point of the product was 92 °C-95 °C (15 mmHg) and the refractive index nD20 was 1.5020.
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Yield: 91%
Reaction Conditions:
with sodium hydroxide in hydrogenchloride;methanol
Steps:
1 EXAMPLE 1
EXAMPLE 1 400 ml of methanol, 20 g of benzyldimethyldodecylammonium chloride and 180 g of 4-chloro-3-nitro-benzotrifluoride are initially introduced into the reaction flask, whilst stirring, and 400 g of 50% strength sodium hydroxide solution are then added dropwise. The temperature rises to about 70° C. if the addition is carried out in the course of about 20 minutes. The mixture is then stirred at 65° C. for a further 4 hours and subsequently cooled by adding ice, and the pH is adjusted to 3 with concentrated hydrochloric acid. The phenol is driven over with steam and the phases are separated in the receiver by adding about 50 ml of concentrated hydrochloric acid. 156 g of 2-nitro-4-trifluoromethylphenol are obtained with a purity of more than 98.5%, according to analysis by gas chromatography, which corresponds to a yield of 91% of theory. Boiling point: 92°-95° C. at 15 mm, nD20: 1.5020.
References:
Bayer Aktiengesellschaft US4225731, 1980, A
121-17-5
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$19.00/250g
400-99-7
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402-45-9
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400-98-6
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400-99-7
182 suppliers
$19.00/5g