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CAS No. : | 17630-75-0 | MDL No. : | MFCD00191927 |
Formula : | C8H6ClNO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WWJLCYHYLZZXBE-UHFFFAOYSA-N |
M.W : | 167.59 | Pubchem ID : | 152801 |
Synonyms : |
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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: |
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* 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 |
---|---|---|
40% | With piperidine; In ethanol; for 8.0h;Heating / reflux; | A mixture of 5-chlorooxindole (6.98 g, 41.6 mmol), 3,5-dimethyl-1H-pyrrole-2-carboxaldehyde (5.12 g, 41.6 mmol) and piperidine (410 muL, 4.16 mmol) in 200 mL of EtOH was heated at reflux for 8 h. The reaction mixture was cooled to room temperature and filtered to give the title compound (4.50 g, 40%) as a red/orange solid. |
40% | With piperidine; In ethanol; for 8.0h;Heating / reflux; | A mixture of 5-chlorooxindole (6.98 g, 41.6 mmol), 3,5-dimethyl-1H-pyrrole-2-carboxaldehyde (5.12 g, 41.6 mmol) and piperidine (410 muL, 4.16 mmol) in 200 mL of EtOH was heated at reflux for 8 h. The reaction mixture was cooled to room temperature and filtered to give the title compound (4.50 g, 40%) as a red/orange solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Scheme III [0139] The process of Scheme III is a multi-step synthetic sequence that commences with the reductive animation of an aniline such as structure 10 with a benzaldehyde and conversion into the chloroacetanilide of structure 11 with chloroacetyl chloride. Palladium catalyzed ring closure gives the N-benzyl oxindole such as structure 12, which is then coupled to the diazonium salt of the biphenyl amino acid of structure 4 to give the final product of structure 9. ; Example 11: 3 '-[N'-( 1 -Benzyl-5 -chloro-2-oxo - 1 ,2-dihvdro-indol-3 -ylidene)-hvdrazino] -T- hydroxy-biphenyl-3-carboxylic acid (Compound 111) [0195] This compound was prepared as described in Scheme III. 1H NMR (500 MHz, DMSCW5) delta 13.10 (s, IH), 13.03 (s, IH), 9.36 (s, IH), 8.13 (t, j =1.7 Hz, IH), 7.95 (ddd, J =7.7, 1.7, 1.3 Hz, IH), 7.80 (ddd, J=7.7, 1.7, 1.3 Hz, IH), 7.76 (dd, J=7.7, 1.6 Hz, IH), 7.68 (d, /=2.1 Hz, EPO <DP n="66"/>IH), 7.60 (t, J=I .1 Hz, IH), 7.37-7.32 (m, 4H), 7.30 (dd, 7=8.5, 2.1 Hz, IH), 7.27 (m, IH), 7.11 (t, J=7.7 Hz, IH), 7.09 (d, J=8.5 Hz, IH), 7.03 (dd, 7=7.7, 1.6 Hz, IH), 5.05 (s, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With piperidine; In methanol; at 100.0℃; for 0.5h;Microwave irradiation; | General procedure: Equimolar amounts (0.3 mmol) of 5-chlorooxindole/oxindole and aldehyde were dissolved in methanol (1 ml), a drop of piperidine (30 μl) was added and the mixture heated at 100C under microwave irradiation for 30 min. The reaction mixture was cooled to room temperature and the resulting precipitate was removed by filtration, carefully washed with methanol and recrystallized at least once from methanol to give the desired product in good yield. |
97% | With pyridine; In methanol; at 100.0℃; for 0.5h;Microwave irradiation; | General procedure: A suspension of indolinone (0.3mmol), aldehyde (0.3mmol) and pyridine (30μL) in methanol (1mL) were heated under microwave irradiation at 100 C for 30 minutes. The reaction mixture was cooled to room temperature and the resulting precipitate was removed by filtration, carefully washed with methanol and dried in vacuo. When no precipitate was observed methanol was removed under vacuum and the residue was purified by silica gel chromatography to give the desired product. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | With piperidine; In ethanol;Reflux; | General procedure: To a mixture of oxindole (3a-f, 0.3mmol), 1-alkyl-1H benzo[d]imidazole-2-carbaldehydes (7a-e, 0.33mmol) in ethanol (2mL), was added catalytic amount of piperidine. The reaction mixture was stirred at reflux until complete consumption of the oxindole observed by TLC. After cooling, the precipitate was filtered, washed with cold ethanol, and dried in air to furnish pure (E)-benzo[d]imidazol-2-yl)methylene)indolin-2-ones 8a-z orange/yellow solids in moderate to good yields. Compounds 8c, 8f, 8i, 8l and 8o did not precipitated out from ethanol, were purified by column chromatography with silica gel (60-120) by using ethyl acetate:hexane (2:8 to 3:7). 4.1.1.7 (E)-5-Chloro-3-((1-methyl-1H-benzo[d]imidazol-2-yl)methylene)indolin-2-one (8g) Orange solid, Yield 81%; mp: 279-281 C; FT-IR: (cm-1): 3157, 3065, 1703, 1608, 1317, 807, 724; 1H NMR (500 MHz, DMSO-d6): δ 10.85 (brs, 1H, NH), 9.68 (d, J = 2.3 Hz, 1H, Ar-H), 7.80 (d, J = 7.9 Hz, 1H, Ar-H), 7.71 (d, J = 8.1 Hz, 1H, Ar-H), 7.63 (s, 1H, C=CH), 7.43-7.31 (m, 3H, Ar-H), 6.91 (d, J = 7.8 Hz, 1H, Ar-H), 4.04 (s, 3H, CH3); 13C NMR (75 MHz, DMSO-d6): δ 168.5, 147.1, 142.5, 142.1, 135.4, 130.5, 129.3, 127.4, 125.2, 124.3, 123.1, 122.4, 119.5, 119.2, 110.8, 110.6, 30.1; HRMS (ESI): m/z calcd for C17H13ClN3O 310.0747, found 310.0743 [M+H]+; Purity: 99.5%. |
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