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CAS No. : | 1135-12-2 | MDL No. : | MFCD00047861 |
Formula : | C13H13N | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | WDTRNCFZFQIWLM-UHFFFAOYSA-N |
M.W : | 183.25 | Pubchem ID : | 136914 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
96% | With pyridine hydrochloride; In 1-ethoxyethanol; | REFERENCE EXAMPLE 9 4-(4-Benzylanilino)-7-bromo-3-quinolinecarbonitrile A mixture of 4-aminodiphenylmethane (604 mg, 3.3 mmol), <strong>[364793-57-7]7-bromo-4-chloro-3-quinolinecarbonitrile</strong> (800 mg, 3.0 mmol) and pyridine hydrochloride (30 mg) in 15 nL of ethoxyethanol was heated at reflux for I hour. The mixture was cooled, poured into 5% sodium carbonate solution, and stirred. The product was filtered, washed with water, and dried to provide 1.20 g (96% yield) of 4-(4-benzylanilino)-7-bromo-3-quinolinecarbonitrile as a tan solid, mp 195-197 C; 1H NMR (DMSO-d6) delta 3.99 (s, 2H), 7.26 (mn, 9H), 7.81 (dd, J=9, 2 Hz, 1H), 8.12 (d, J=2 Hz, 1H), 8.41 (d, J=9 Hz, 1H), 8.57 (s, 1H), 9.91 (s, 1H); MS (ES) m/z 416.1 (M+1). Analysis for C23Hl6 BrN3: Calcd: C, 66.68;H, 3.89; N, 10.14. Found: C, 66.67;H, 3.96; N, 9.81. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | In 1,4-dioxane; at 20 - 85℃; | To a solution of Ethyl-4,6-dichloroquinoline-3-carboxylate (1.0 g, 3.7 mmol) in 1,4-dioxane (10 mL) was added a solution of 4-benzylbenzenamine (733 mg, 4.0 mmol) in 1,4-dioxane (10 mL) at room temperature. After stirred at 85 C 1 hour, the reaction mixture was then cooled down to room temperature and then treated with 20 mL of water. The resulting suspension treated with 10 NNaOH solutions to reach the pH about 9. It was partitioned between ethyl acetate and water. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over MgSO4, filtered and concentrated. The crude product was purified by flash column chromatography using a 9:1 v/v hexane: ethyl acetate as solvent to afford title compound (1.1 g, 65 % yield) as a yellow solid.[00209] 1H NMR 600 MHz (DMSO-fc) delta 9.69 (s, 1H), 8.12 (d, J = 2.1 Hz, 1H), 7.91(d, J = 8.8 Hz, 1H), 7.74 (dd, J= 2.1, 6.7 Hz, 1H), 7.46 (m, 1H), 7.24 (m, 3H), 7.16 (m, 3H), 7.00 (d, J= 8.2 Hz, 2H), 3.90 (s, 2H), 3.86 (s, 1H), 3.84 (q, J= 7.0 Hz, 2H), 1.03 (/, J= 7.3 Hz, 3H), MS m/z 417.36 (M + 1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Dissolved 0.500 g <strong>[17823-69-7]2-cyano-3,3-bis(methylthio)acrylamide</strong> in 15 mL EtOH and added 4-Aminodiphenylmethane (1.0 eq.) . Stirred reaction at 75 C until starting amide was absent by HPLC. Once complete (18 hrs), reaction was brought to room temperature and filtered to obtain a light yellow powder as product. Product was allowed to dry under vacuum for 1 hr. Product was then suspended in 10 mL EtOH and hydrazine hydrate (1 eq.) was added dropwise. Reaction was heated at 75 C until intermediate was absent (HPLC). Once intermediate was absent (18 hrs), reaction was brought to room temperature and filtered to obtain a yellow powder as product. Product was allowed to dry under vacuum for 1 hr. 5-amino-3-((4-benzylphenyl)amino)-lH-pyrazole-4-carboxamide |
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