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White, Robert H. ; Allen, Kylie D. ; Wegener, Gunter ACS Omega,2019,4(27):22613-22622. DOI: 10.1021/acsomega.9b03450 PubMed ID: 31909345
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Abstract: The anaerobic oxidation of methane (AOM) mitigates the flux of methane from marine sediments into the water column. AOM is performed by anaerobic methanotrophic archaea (ANME) that reverse the methanogenesis pathway and partner bacteria that utilize the released reducing equivalent for sulfate reduction We investigated small-mol. extracts from sediment-free thermophilic enrichment cultures of ANME-1 and sulfate-reducing bacteria using ultraperformance liquid chromatog. with high-resolution mass spectrometry. During the anal., we discovered a novel thioquinoxalinol-containing redox mol. as a major component of the chem. derivatized small-mol. pool. This compound contains both a redox active quinoxaline heterocyclic ring and a thiol group. Addnl., the same structure was identified that contains a sulfate ester on the hydroxyl group, which likely makes the mol. more water soluble Hydrated versions of both structures were also observed as major compounds in the extracts On the basis of reactions of model compounds such as quinoxalin-6-ol, the hydrated version appears to be formed from the addition of water to the dehydropyrazine ring followed by an oxidation These thioquinoxalinol compounds, which represent completely new structures in biochem., may be involved in electron transport processes within and(or) between ANME-1 and sulfate-reducing bacteria, may serve protective roles by reacting with toxic compounds such as hydrogen sulfide, or may transport sulfate as a sulfate ester into the sulfate-reducing bacteria.
Purchased from AmBeed: 122-57-6 ; 15529-49-4
CAS No. : | 122-57-6 | MDL No. : | MFCD00008779 |
Formula : | C10H10O | Boiling Point : | - |
Linear Structure Formula : | CH3C(O)CHCHC6H5 | InChI Key : | BWHOZHOGCMHOBV-BQYQJAHWSA-N |
M.W : | 146.19 | Pubchem ID : | 637759 |
Synonyms : |
Benzalacetone
|
Chemical Name : | 4-Phenylbut-3-en-2-one |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P270-P272-P280-P301+P312-P302+P352-P305+P351+P338-P333+P313-P337+P313-P362+P364-P403-P501 | UN#: | N/A |
Hazard Statements: | H302-H315-H317 | 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 |
---|---|---|
94% | With tetrabutylammomium bromide; toluene-4-sulfonic acid hydrazide; sodium hydroxide; In water; at 80℃; for 10h;Air atmosphere; | General procedure: A Schlenk tube with a magnetic stir bar charged with alpha,beta-unsaturated carbonyl compounds (0.5 mmol, 1 equiv), tosyl hydrazide (0.6 mmol, 1.2 equiv), NaOH (1.5 equiv), (n-Bu)4NBr (1.5 equiv). The reaction vessel was placed in an 80 C oil bath, and then stirring at this temperature for 10 h. The reaction mixture was then allowed to cool to ambient temperature, and diluted with 20 mL of ethyl acetate, and washed with brine (15 mL), water (15 mL), and then the organic layer was dried over Na2SO4. After concentrated in vacuo, the crude product was purified by column chromatography. The identity and purity of the known product was confirmed by 1H NMR, 13C NMR, and GC-MS. |
81% | With iodine; potassium carbonate; toluene-4-sulfonic acid hydrazide; In ethanol; at 75℃; for 2h;Green chemistry; | General procedure: To a stirred mixture of alpha,beta-unsaturated aldehydes/ketones 1 (0.5 mmol) and TsNHNH2 (0.6 mmol) in EtOH (2.0 ml) was added molecular iodine (2.5 mg, 2 mol%) in an oven-dried flask, and then the reaction was heated to 75 C for 10 min followed by the addition of K2CO3 immediately. The reaction proceeded under an air atmosphere for 1.5-2.0 h until complete consumption of starting material as monitored by TLC. The reaction mixture was concentrated under vacuum and the crude product was purified by column chromatography using petroleum ether/ethyl acetate as eluent to provide the product 2. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With ammonium acetate; In ethanol; at 80℃; for 4h;Microwave irradiation; | To a solution of the dinitropyridone 1 (50 mg, 0.25 mmol) in ethanol (10 mL), 4-phenyl-3-buten-2-one (4a) (36.5 mg, 0.25 mmol) and NH4OAc (578 mg, 7.5 mmol) were added, and the resultant mixture was heated at 65 C for 24 h. After removal of the solvent, the residue was washed with benzene (3 × 10 mL) to remove unreacted ketone 4a and treated with column chromatography on silica gel (eluent: hexane/ethyl acetate =95/5) to afford 5-nitro-2-(2-phenylethenyl)pyridine (5a) (41 mg, 0.18 mmol, 72%) as a yellow powder. The reactions of the dinitropyridone 1 with other ketones 4b-f or 10a-c were performed in a similar way. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
73% | With 1,4-diaza-bicyclo[2.2.2]octane; In water; at 80℃; for 1.5h; | General procedure: To a stirred mixture of isatin (1a) (200 mg, 1.36 mmol) in 10 mL of water, benzalacetone (2a) (198 mg, 1.36 mmol) and DABCO (152 mg, 1.36 mmol) were added and reaction mixture allowed to stir vigorously at 80C for 1.5 hours. After the TLC indicated complete consumption of starting material, the reaction mixture was filtered and product 3a was collected as white solid. |
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