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CAS No. : | 22445-41-6 | MDL No. : | MFCD00060659 |
Formula : | C8H9I | Boiling Point : | - |
Linear Structure Formula : | IC6H3(CH3)2 | InChI Key : | ZLMKEENUYIUKKC-UHFFFAOYSA-N |
M.W : | 232.06 | Pubchem ID : | 140924 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
15%Chromat. | With N,N`-dimethylethylenediamine;copper(l) iodide; In toluene; at 110℃; for 24h; | Schlenk tube was charged with CuI (19.5 mg, 0.102 mmol, 20 mol%), KCN (78 mg, 1.20 mmol), evacuated, backfilled with Ar. N, N'-Dimethylethylenediamine (21. 5 [UL,] 0.202 mmol, 20 mol%), 5-bromo-m-xylene (136 [PL,] 1.00 mmol), and toluene (1.0 mL) were added under Ar. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 110 [C] for 24 h. Dodecane (internal GC standard, [230] [GEL),] ethyl acetate (2 mL), and 30% aq ammonia (1 mL) were added. A 0.1 mL sample of the supernatant solution was diluted with ethyl acetate (1 mL) and analyzed by GC to provide a 15% yield of 3, 5-dimethylbenzonitrile. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With silver(I) acetate; palladium diacetate; acetic acid; at 50℃; for 12h; | General procedure: A mixture of 1a (79 mg, 0.5 mmol), iodobenzene (112 mg, 1.1 equiv), Pd(OAc)2 (6 mg, 5 mol%), AgOAc (92 mg,1.1 equiv), and AcOH (1.5 g, 50 equiv) was heated to 50 C for 5 h. After the aqueous extractive workup and column chromatographic purification process (hexanes/Et2O, 20:1), the product 2a was isolated as a colorless oil, 101 mg (86%). Other compounds were synthesized similarly, and the selected spectroscopic data of unknown compounds 2b, 2e-meta, 2e-ortho, 2h, 3a, 3emeta, 3f, and 3i are as follows. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | With [ruthenium(II)(eta6-1-methyl-4-isopropyl-benzene)(chloride)(mu-chloride)]2; potassium carbonate; triphenylphosphine; In benzene; at 150℃; for 24h;Sealed tube; | General procedure: In a 30-mL sealed tube, <strong>[2622-63-1]1-methyl-2-phenylbenzimidazole</strong> (1, 0.25mmol), [RuCl2(p-cymene)]2 (0.0125 mmol), Ph3P (0.075 mmol),K2CO3 (0.50 mmol), and iodoarene (0.25 mmol) were combined inanhydrous benzene (2 mL) under air. The mixture was then stirredat 150 °C for 24 h. The mixture was cooled to r.t., diluted with EtOAc, and filtered through a small pad of Celite. The filtrate was concentrated in vacuo and purified by flash chromatography (silicagel, EtOAc?hexane) to give the analytically pure 2-(biphenyl-2-yl)benzimidazoles. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With potassium phosphate; In N,N-dimethyl-formamide; at 120℃; for 1h; | General procedure: Aryliodide (0.5 mmol), K4[Fe(CN)6]3H2O(0.15 mmol), K3PO4 (1.5 mmol) and Pd-BNP (5.3 mg, 0.005 mmol, 1.0 mol%)were taken in a oven dried reaction tube equipped with magnetic pellet. DMF(2.0 mL) was added to the reaction tube and the reaction mixture was stirred at120 C temperature. The reaction was monitored by TLC. After consumption ofthe starting material, the reaction mixture was cooled to room temperature.Crude product was extracted with ethyl acetate (3 10 mL). Then the organicphase was dried over Na2SO4 and concentrated in vacuum. The product waspurified by column chromatography using silica gel. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With copper (II) trifluoroacetate hydrate; palladium diacetate; In dimethyl sulfoxide; at 130℃; for 6h;Sealed tube; Inert atmosphere; | General procedure: Aryl iodide (0.7 mmol, 1 equiv), tert-butyl isocyanide (2.1 mmol, 237 muL, 3 equiv), Pd(OAc)2 (0.035 mmol, 8 mg, 5 mol %), Cu(TFA)2*xH2O (1.4 mmol, 405 mg, 2 equiv) and DMSO (2.5 mL) were added to a 15 mL sealed tube, and stirred at 130 C for 4-12 h under nitrogen. After completion of the reaction indicated by TLC, the mixture was extracted with Et2O (510 mL). The combined organic phases was dried over Na2SO4, and concentrated under vacuum. Then the residue was purified by column chromatography on silica gel using petroleum ether (30-60 C)/Et2O as eluant to provide the pure target product. |
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