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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
Limited Quantity | USD 15-60 |
Inaccessible (Haz class 6.1), Domestic | USD 80+ |
Inaccessible (Haz class 6.1), International | USD 150+ |
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CAS No. : | 34857-66-4 | MDL No. : | MFCD20483811 |
Formula : | C8H4ClF3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 224.56 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 6.1,8 |
Precautionary Statements: | P501-P260-P270-P262-P234-P271-P264-P280-P284-P390-P361+P364-P303+P361+P353-P301+P330+P331-P301+P310+P330-P304+P340+P310-P305+P351+P338+P310-P403+P233-P406-P405 | UN#: | 3277 |
Hazard Statements: | H300+H310+H330-H314-H290 | Packing Group: | Ⅱ |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | With potassium carbonate; In acetone; | EXAMPLE 3 Preparation of 4-trifluoromethylphenyl N-(6-methoxy-2-pyridyl)-N-methylcarbamate (Compound No. 97) To the mixture of 1.38 g of <strong>[88569-83-9]2-methoxy-6-methylaminopyridine</strong> and 1.38 g of anhydrous potassium carbonate in 20 ml of acetone was added dropwise the solution of 2.25 g of 4-trifluoromethylphenyl chloroformate in 20 ml of acetone under stirring at room temperature. The mixture was stirred for 30 minutes and then was refluxed for 2 hours. After the reaction mixture was cooled to room temperature, it was poured into water and the product was extracted with benzene. The benzene solution, successively washed with water and brine, was dried over anhydrous magnesium sulfate. The residue obtained by the removal of benzene under reduced pressure was chromatographed through silica gel column using benzene as an eluent to give 2.02 g of pure 4-trifluoromethylphenyl N-(6-methoxy-2-pyridyl)-N-methylcarbamate as solid in the yield of 62%. A part of the solid was recrystallized from hexane and crystalls having melting point of 85 to 86 C. were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: sodium azide / acetone / 12 h / 20 °C 2: C19H19Cl3CoNO; sodium tetrakis[(3,5-di-trifluoromethyl)phenyl]borate / 12 h / 40 °C / Sealed tube |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1.295 g | With triethylamine In tetrahydrofuran at 0℃; for 1h; Inert atmosphere; | 4-(Trifluoromethyl)phenyl 3-methyl-2-(((4-(trifluoromethyl)phenoxy)carbonyl)oxy)-1Hindole-1-carboxylate (1Ca) To a solution of 3-methyl-2-oxindole (0.741 g, 5.03 mmol) in THF(15 mL) were added Et3N (1.242 g, 12.2 mmol) and 4-(trifruolomethyl)phenyl chloroformate(2.695 g, 12.0 mmol) at 0 °C. The mixture was stirred at 0 °C for 1 h, then poured into water, andextracted with Et2O. The combined organic layer was washed with 1 N hydrochloric acid,saturated aqueous NaHCO3, and brine, and dried over MgSO4. After filtration and concentration,the residue was purified by silica gel column chromatography (hexane:Et2O = 1:1) to give 1Caas a colorless solid (1.295 g, 50%). 1H NMR (400 MHz, CDCl3, δ): 8.10 (d, J = 7.4 Hz, 1H), 7.75(d, J = 8.3 Hz, 2H), 7.65 (d, J = 8.6 Hz, 2H), 7.57-7.54 (m, 1H), 7.44 (d, J = 8.9 Hz, 2H), 7.43-7.34 (m, 2H), 7.30 (d, J = 8.6 Hz, 2H), 2.29 (s, 3H). 13C NMR (100 MHz, CDCl3, δ): 153.3, 152.4,150.9, 148.1, 137.0, 132.1, 129.3 (q, J = 33.0 Hz), 129.2 (q, J = 33.0 Hz), 128.3, 127.3 (q, J = 3.9Hz), 127.2 (q, J = 3.9 Hz), 125.7, 124.3, 123.9 (q, J = 272 Hz), 123.8 (q, J = 272 Hz), 122.3,121.4, 119.5, 115.7, 107.3, 7.2. 19F NMR (376 MHz, CDCl3, δ): -63.3, -63.4. HRMS-APCI (m/z):[M + H]+ calcd for C25H15F6NO5, 524.0927; found, 524.0935. |