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CAS No. : | 120277-14-7 | MDL No. : | MFCD11520709 |
Formula : | C6H5BrFN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 190.01 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P260-P264-P270-P280-P301+P330+P331-P303+P361+P353-P304+P340-P305+P351+P338-P310-P363-P405-P501 | UN#: | 3261 |
Hazard Statements: | H302-H314 | 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 |
---|---|---|
With potassium carbonate In N,N-dimethyl-formamide at 20℃; | Compound 12: 2,2-difluoro-4-[(5-fluoro-3-pyridinyl)methyl]-8-[(1/?)-2,2,2-trifluoro-1 - hydroxyethyl]-2H-1 ,4-benzoxazin-3(4H)-one and compound 13: 2,2-difluoro-4-[(5- fluoro-3-pyridinyl)methyl]-8-[(1 S)-2,2,2-trifluoro-1-hydroxyethyl]-2H-1,4-benzoxazin- 3(4H) -oneR-stereoisomer S-stereoisomer2.2-Difluoro-8-(2.2,2-trifluoro-1-hydroxyethyl)-2H-1 ,4-benzoxazin-3(4H)-one (105 mg, 0.369 mmol; may be prepared as described in intermediate 5), 3-(bromomethyl)-5- fluoropyridine (100 mg; Sunshine Chemicals) and potassium carbonate (102 mg) were dissolved in DMF (5000 μl) in a 10 ml. round-bottomed flask open to the atmosphere and stirred at RT overnight. The reaction mixture was evaporated to dryness, redissolved in EtOAc (30 ml) and treated with saturated aqueous sodium bicarbonate solution (30 ml). The aqueous layer was extracted with EtOAc (2 x 30 ml) and the organic layers were combined, washed with brine (30 ml), dried over magnesium sulfate, filtered and evaporated to dryness to give the crude product (160 mg) as a colourless oil. The crude product was purified on a 25+S Biotage silica cartridge, eluting with a 0 to 75 % mixture of EtOAc in hexane. This gave the target compound (racemate) (94 mg) as a white solid. 83 mg of this racemic mixture was separated into its constituent enantiomers by chiral preparative HPLC (Chiralpak AD column eluting with heptane: ethanol (70:30) v/v pump- mixed) to give the faster-running enantiomer as a white solid and the slower-running enantiomer as a white solid. These compounds were purified on 12+M Biotage silica cartridges, eluting with 0 to 75 % mixtures of EtOAc in hexane. This gave the faster- running enantiomer as a white solid and the slower-running enantiomer (22 mg, compound 12 or 13) as a white solid. The faster-running enantiomer was purified again by MDAP to give the faster-running enantiomer (12 mg, compound 12 or 13) as a white solid. 1H NMR (CD3OD) δ: 4.52 (2H, q), 4.62 (1 H, q), 6.40 - 6.45 (2H, m), 6.63 (1 H, q), 6.70 (1 H, dt), 7.51 - 7.55 (2H, m). m/z [M+H]+: 393.2. Retention time 0.98 min (LC/MS method 3). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
6% | Stage #1: (S)-methyl 2-(3-hydroxypyrrolidin-1-yl)-5-(trifluoromethyl)benzoate With sodium hydride In N,N-dimethyl-formamide; mineral oil at 0℃; for 1h; Stage #2: 3-(bromomethyl)-5-fluoropyridine In N,N-dimethyl-formamide; mineral oil at 0 - 50℃; for 22h; | 15 (S)-Methyl 2-(3-hydroxypyrrolidin-1-yl)-5-(trifluoromethyl)benzoate (11b) General procedure: To a solution of 11b (1.50 g, 5.18 mmol) in DMF (20 mL) was added NaH (60% in mineral oil w/w, 0.23 g, 5.75 mmol) in small portions at 0 °C. The reaction mixture was stirred at 0 °C for 1 h, 2-cyclopropylethyl 4-methylbenzenesulfonate, (1.60 g, 6.65 mmol) was added; stirring was continued for 18 h and then heated at 50 °C for 4 h. The reaction mixture was quenched by addition of aqueous saturated NH4Cl solution (10 mL) at 0 °C and extracted with ethyl acetate (100 mL x 3), washed with water and brine' dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo, the residue was subjected to column chromatography with a gradient of 10-30% EtOAc in hexanes to give 11c as a colorless oil (1.76 g, 95%). 1H NMR (300 MHz, CDCl3) δ 7.83-7.79 (m, 1H), 7.50-7.45 (m, 1H), 6.80-6.75 (m, 1H), 4.14-4.08 (m, 1H), 3.88 (s, 3H), 3.58-3.38 (m, 4H), 3.36-3.28 (m, 1H), 3.08-3.00 (m, 1H), 2.16-2.00 (m, 2H), 1.43-1.35 (m, 2H), 0.69-0.59 (m, 1H), 0.41-0.35 (m, 2H), 0.19-0.03 (m, 2H); MS (ES+) m/z 358.1 (M+1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: sodium hydride / N,N-dimethyl-formamide; mineral oil / 1 h / 0 °C 1.2: 22 h / 0 - 50 °C 2.1: sodium hydroxide; water / tetrahydrofuran / 18 h / Reflux |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine In dichloromethane at 20℃; for 2h; |