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With sulfuric acid; nitric acid; at 90℃; for 1.18333h;
Preparation of 2-chloro-3-nitro-5-trifluoromethylbenzoic acid [Show Image]2-Chloro-5-trifluoromethylbenzoic acid (6.5044 g, 28.965 mmol) was added to a solution of sulfuric acid (23 mL) and fuming nitric acid (3.2 mL), with an overhead stirring. The mixture was warmed to 90C over 26 min then a further 10 mL of sulfuric acid was added to the thick mixture and stirring was continued. After 45 min at 90C the mixture was cooled to ambient temperature and poured into crushed ice (150 g), rinsing forward with icy water (50 mL). The product was isolated by vacuum filtration, washed with cold water, and dried in vacuo to give 7.3752 g (94.7 %). LCMS: Rt = 5.74 min, 100 A% (at) 254 nm, [M-H]- = 268.0. Co- injection of the product and starting material revealed the compounds were baseline separated.
94.7%
With sulfuric acid; nitric acid; at 90℃; for 1.18333h;
2-Chloro-5-trifluoromethylbenzoic acid (6.5044 g, 28.965 mmol) was added to a solution of sulfuric acid (23 mL) and fuming nitric acid (3.2 mL), with an overhead stirring. The mixture was warmed to 90C over 26 min then a further 10 mL of sulfuric acid was added to the thick mixture and stirring was continued. After 45 min at 90C the mixture was cooled to ambient temperature and poured into crushed ice (150 g), rinsing forward with icy water (50 mL). The product was isolated by vacuum filtration, washed with cold water, and dried in vacuo to give 7.3752 g (94.7 %). LCMS: Rt = 5.74 min, 100 A% (at) 254 nm, [M-H]- = 268.0. Co-injection of the product and starting material revealed the compounds were baseline separated.
94.7%
With sulfuric acid; nitric acid; at 90℃; for 1.18333h;
2-Chloro-5-trifluoromethylbenzoic acid (6.5044 g, 28.965 mmol) was added to a solution of sulfuric acid (23 mL) and fuming nitric acid (3.2 mL) , with an overhead stirring. The mixture was warmed to 90 C over 26 min, then a further 10 mL of sulfuric acid was added to the thick . mixture and stirring was continued. After 45 min at 90 C the mixture was cooled to ambient temperature and poured into crushed ice (150 g) , rinsing forward with icy water (50 mL) . The product was isolated by vacuum filtration, washed with cold water, and dried in vacuo to give 7.3752 g (94.7 %) . LCMS: Rt = 5.74 min, 100 A% (at) 254 nm, [M-H] " = 268.0. Co- injection of the product and starting material revealed the compounds were baseline separated.
81.1%
With fuming sulphuric acid; sulfuric acid; nitric acid; at 0 - 60℃; for 1.5h;
2-chloro-5-trifluoromethylbenzoic acid (8.98 g, 40 mmol) was dissolved in 14.4 mL of concentrated sulfuric acid. Stir until completely dissolved,to the reaction solution, fuming sulfuric acid (50%) 9.6 mL was added. cool in ice bath to 0 C, Slowly add 7.0 mL of fuming nitric acid to the reaction system. Keeping the temperature of the reaction system below 60 C during the dropwise addition, After 30 minutes, After stirring for 1 hour, Add ice water 150mL, Precipitated in white, Filtration, washing with water and drying to give the intermediate 2-chloro-3-nitro-5-(trifluoromethyl)benzoic acid 1a. The white solid was 8.73 g, yield 81.1%.
With sulfuric acid; sulfur trioxide; nitric acid; at 20 - 60℃; for 0.5h;
Example 1: N-(3,4-Dichlorophenyl)-3-nitro-2-piperid-1-yl-5- triflupsilonoromethylbenzamide.Step a): 2-Chloro-3-nitro-5-trifluoromethylbenzoic acid.After dissolving at room temperature 2-chloro-5-trifluoromethylbenzoic acid (2.25 g; 10 mmol) in fuming sulfuric acid comprising 20% oleum (6 ml), fuming nitric acid (1.7 ml) is added dropwise over 30 minutes, so as to maintain the temperature of the reaction medium below 600C. After cooling, ice is added and the precipitate is separated out, washed with water and dried. After recrystallisation from water, 2.15 g of solid corresponding to 2-chloro-3-nitro-5-trifluoromethylbenzoic acid are obtained (m.p. = 173C).1H NMR (300 MHz, CDCI3) delta ppm: 8.41 (d, 1H), 8.71 (d, 1 H), 14.30 (s, 1H)
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