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CAS No. : | 127733-40-8 | MDL No. : | MFCD03093013 |
Formula : | C10H9F6N | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | PFVWEAYXWZFSSK-YFKPBYRVSA-N |
M.W : | 257.18 | Pubchem ID : | 1512509 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
5%-palladium/activated carbon; In methanol; at 60℃; under 1500.15 Torr; for 22.0h;Heating; | 13.3 g (24.95 mmol, 1 eq) of the p-toluenesulfonate of optically active secondary amine (4a) purified with reference to Example 36 (4a.p-toluenesulfonate, 99.6% de, major form: S-S form) and 100 ml (50 mmol, 2 eq) of 0.5 N aqueous NaOH were added to 50 ml of toluene, followed by stirring for 30 minutes at room temperature, separating statically, extracting the recovered aqueous layer with toluene, washing the combined recovered organic layers with saturated brine, drying with an hydrous sodium sulfate, filtering, concentrating and vacuum drying to obtain an optically active secondary amine (4a) having the structure indicated below at the quantitative yield. [C00047] [00196] The resulting 4a was dissolved in 26 ml of methanol, followed by the addition of 0.45 g (0.125 wt %) of 5% palladium/active carbon (water content: 50 wt %), setting the hydrogen pressure to 0.2 MPa and stirring for 22 hours at 60 C. Following completion of the reaction, the reaction liquid was filtered with Celite, concentrated and vacuum dried to obtain a crude product of optically active 1-(3, 5-bis-trifluoromethylphenyl)ethylamine (5a) having the structure indicated below at the quantitative yield. The crude product was purified by simple distillation (96-97 C./31 mmHg) to obtain 5.41 g of a highly pure product (total yield for the two steps: 84%). GC purity and ee were 99.4% and 99.4% ee, respectively. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In acetonitrile; | EXAMPLE 91(.) N-(5-[({(1 S)-1-[3,5-bis(trifluoromethyl)phenyl]ethyl}amino)carbothioyl]amino}-2-pyridinyl)-1,3-thiazole-4-carboxamide A mixture of N-(5-isothiocyanato-2-pyridinyl)-1,3-thiazole-4-carboxamide (0.36 g) and (S)-alpha-methyl-3,5-bis(trifluoromethyl)-benzenemethanamine (0.36 g) is heated with acetonitrile (10 mL) until all solids are dissolved. The solution is allowed to stand for 12 hours. A white solid forms and is collected by filtration (0.40 g). [M+H] 520. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In hexane; toluene; at 20 - 70℃; for 24.5h; | 1.02 g (3.97 mmol, 1 eq) of optically active 1-(3,5-bis-trifluoromethylphenyl)ethylamine (5a, enantiomer ratio/S form:R form=7.4:1) and 0.68 g (3.59 mmol, 0.9 eq) of p-toluenesulfonic acid monohydrate were added to 6.5 ml of toluene, followed by stirring for 30 minutes at 60-70 C., the addition of 6 ml of n-hexane and allowing to cool to room temperature and stand for one day. The precipitated crystals were filtered, washed with a small amount of n-hexane and vacuum dried to obtain 0.20 g of crystals having the structure represented by the formula below and 1.44 g of mother liquor. They were converted to the free bases with 0.5 N aqueous NaOH and analyzed by chiral GC. With this, respective ee were found to be 82.7% ee (major form is the S form) and 74.2% ee (major form is the S form). [C00039] [00180] 1H-NMR (TMS, DMSO): 1.54 (d, 6.8 Hz, 3H), 2.28 (s, 3H), 4.69 (q, 6.8 Hz, 1H), 7.10 (d, 8.3 Hz, 2H), 7.46 (d, 8.3 Hz, 2H), 8.17 (s, 1H), 8.23 (s, 2H), 8.30 (br, 31). |
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