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Type
HazMat fee for 500 gram (Estimated)
Excepted Quantity
USD 0.00
Limited Quantity
USD 15-60
Inaccessible (Haz class 6.1), Domestic
USD 80+
Inaccessible (Haz class 6.1), International
USD 150+
Accessible (Haz class 3, 4, 5 or 8), Domestic
USD 100+
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USD 200+
Structure of 2632-10-2 * Storage: {[proInfo.prStorage]}
* 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.
With N-Bromosuccinimide; toluene-4-sulfonic acid In acetonitrile at 80℃; for 5 h;
To a solution of compound ii-c-2 (18.8 g, 0.1 mol, 1.0 eq.) in acetonitrile (100 ml) was added p-toluenesulfonic acid (25.8 g, 0.15 mol, 1.5 eq.)And N-bromosuccinimide (17.7 g, 0.1 mol, 1.0 eq.),The reaction solution was refluxed at 80 ° C for 5 h.The organic phase was extracted and concentrated, and the title compound ii-2 (yield 95percent) was obtained by silica gel column chromatography.
157 g
at 17 - 20℃; for 0.5 h;
To a stirred solution of 3,4-dichloroacetophenone, 135 g (0.714 mol) in acetic acid (675 mL) cooled to 17 °C was added bromine, 37.0 mL (0.722 mol) in acetic acid (360 mL) dropwise. After approximately a third of the bromine had been added no reaction had occurred therefore the reaction mixture was warmed to 25 °C at which point an exotherm to 35 °C occurred. The remainder of the bromine was added and the reaction mixture stirred at room temperature for 30 minutes. The mixture was poured into ice water (1.5 L) while stirring vigorously. The precipitate was collected by filtration and the two batches combined and washed with water. The solid was triturated in diethyl ether (300 mL) to give the desired product 2-bromo-l-(3,4-dichlorophenyl)ethanone, 230 g. The filtrate was washed with brine, dried over magnesium sulfate and concentrated to give a brown oil. The oil was poured into ice/water (1 L) and stirred. The precipitate was collected by filtration to give a second batch of the desired product, 157 g, which were used directly without further purification. ‘HNMR (400 MHz, DMSO-d6): δ [ppm] = 4.95 (s, 2H), 7.81 (d, 1H), 7.91 (dd, 1H), 8.18 (d, 1H). LC (method 1): Rt 2.82 min
Reference：
[1] Russian Journal of Organic Chemistry, 1994, vol. 30, # 6.1, p. 881 - 887[2] Zhurnal Organicheskoi Khimii, 1994, vol. 30, # 6, p. 827 - 832
[3] Patent: CN107266388, 2017, A, . Location in patent: Paragraph 0098; 0099; 0100
[4] ChemMedChem, 2018, vol. 13, # 11, p. 1102 - 1114
[5] Bioorganic and Medicinal Chemistry, 2006, vol. 14, # 21, p. 7146 - 7153
[6] Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry, 2009, vol. 48, # 10, p. 1424 - 1430
[7] ACS Medicinal Chemistry Letters, 2016, vol. 7, # 7, p. 686 - 691
[8] Roczniki Chemii, 1933, vol. 13, p. 293,295[9] Chem. Zentralbl., 1933, vol. 104, # II, p. 1516
[10] Chemische Berichte, 1936, vol. 69, p. 921,924
[11] Journal of the Chemical Society, 1951, p. 255
[12] Journal of medicinal chemistry, 1972, vol. 15, # 9, p. 989 - 994
[13] Chemical and Pharmaceutical Bulletin, 1992, vol. 40, # 5, p. 1170 - 1176
[14] Journal of Medicinal Chemistry, 1998, vol. 41, # 26, p. 5150 - 5157
[15] Journal of the Chemical Society - Perkin Transactions 1, 1999, # 17, p. 2421 - 2423
[16] Journal of agricultural and food chemistry, 2002, vol. 50, # 12, p. 3486 - 3490
[17] Journal of the American Chemical Society, 2004, vol. 126, # 6, p. 1634 - 1635
[18] Synthetic Communications, 2007, vol. 37, # 2, p. 199 - 207
[19] Patent: US5212197, 1993, A,
[20] Patent: US4185105, 1980, A,
[21] Bioorganic and Medicinal Chemistry, 2009, vol. 17, # 17, p. 6374 - 6379
[22] Chemistry and Biodiversity, 2010, vol. 7, # 7, p. 1717 - 1727
[23] Letters in Drug Design and Discovery, 2011, vol. 8, # 9, p. 758 - 762
[24] Letters in Drug Design and Discovery, 2011, vol. 8, # 9, p. 758 - 762
[25] European Journal of Medicinal Chemistry, 2012, vol. 52, p. 70 - 81
[26] Tetrahedron, 2013, vol. 69, # 31, p. 6392 - 6398
[27] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 24, p. 6764 - 6768
[28] RSC Advances, 2014, vol. 4, # 5, p. 2177 - 2194
[29] ChemMedChem, 2014, vol. 9, # 1, p. 177 - 188
[30] Advanced Synthesis and Catalysis, 2013, vol. 355, # 18, p. 3570 - 3574
[31] Chemical Communications, 2014, vol. 50, # 51, p. 6726 - 6728
[32] Drug Design, Development and Therapy, 2016, vol. 10, p. 1807 - 1815
[33] Phosphorus, Sulfur and Silicon and the Related Elements, 2016, vol. 191, # 8, p. 1166 - 1173
[34] Patent: WO2016/91845, 2016, A1, . Location in patent: Page/Page column 55
[35] Organic and Biomolecular Chemistry, 2016, vol. 14, # 34, p. 8026 - 8029
[36] Patent: CN105315279, 2016, A, . Location in patent: Paragraph 0136
[37] Patent: CN105669586, 2016, A, . Location in patent: Paragraph 0050
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2
[ 17356-08-0 ]
[ 2642-63-9 ]
[ 2632-10-2 ]
Reference：
[1] Drug Design, Development and Therapy, 2016, vol. 10, p. 1807 - 1815
3
[ 95-50-1 ]
[ 2632-10-2 ]
Reference：
[1] Journal of the Chemical Society, 1951, p. 255
4
[ 2632-10-2 ]
[ 17356-08-0 ]
[ 39893-80-6 ]
Reference：
[1] Journal of Medicinal Chemistry, 2013, vol. 56, # 22, p. 9031 - 9044
[2] Phosphorus, Sulfur and Silicon and the Related Elements, 2010, vol. 185, # 1, p. 103 - 109
[3] European Journal of Medicinal Chemistry, 2012, vol. 52, p. 70 - 81
[4] Journal of the Chinese Chemical Society, 2017, vol. 64, # 12, p. 1408 - 1416
General procedure: Small amount of 2-bromoacetophenone (1.00 g, 5.02 mmol) was first dissolved in 15 mL of acetone, and 0.39 g (6.03 mmol) of sodium azide was added, and then kept at room temperature for 2 h. After the reaction was completed, the reaction mixture was diluted with 20 mL of ethyl acetate, washed with water, dried over anhydrous magnesium sulfate, and finally concentrated under a reduced pressure. The residues were purified using silica gel column chromatography (hexane : ethyl acetate=10 : 1) to obtain the 2-azido-1-phenylethan-1-one (0.66 g, 82%).
1-(3,4-dichlorophenyl)-2-(phenylsulfonyl)ethan-1-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In N,N-dimethyl-formamide; at 20℃; for 12h;Sealed tube;
General procedure: A sealed tube (35 mL) equipped with a stirring bar was loaded with 2-bromoethanones (1.0 mmol), then sodium benzenesulfinate (1.2 mmol) in DMF (20 mL) or phosphite (1.0 mmol) in toluene (20 mL) was added to the tube and the mixtures were stirred at room temperature till the 2-bromoethanones was totally consumed as indicated by TLC analysis (ca. 12 h for 1 and 24 h for 3). Then, the mixture was diluted with water (20 mL) and extracted with CH2Cl2 (30 mL x 3). Next, the organic phase was combined and dried over anhydrous Na2SO4. The solvent was removed by rotary evaporation and the oily mixture was purified with flash chromatograph column (elute: mixture of ethyl acetate and n-hexane), giving the desired products. And the 1H NMR spectra of the purified substrates were in accordance with the known literatures.
In ethanol; water;Reflux;
General procedure: In a 50 mL round-bottomed flask, a solution of sulfonylchloride (6 mmol) in H2O (25 mL) was prepared, sodiumbicarbonate (0.840 g, 10 mmol) and sodium sulfite (1.26 g,10 mmol) were added, and the mixture was refluxed forabout 4-7 h. The progress of the reaction was monitored byTLC (eluent: n-hexane/ethyl acetate). When the starting materialdisappeared completely, an ethanolic solution of appropriate2-bromoacetophenone (2 mmol) was added to thereaction mixture and heating was continued until the completionof reaction which was monitored by TLC. After cooling,the reaction mixture was neutralized by adding 5% HCl. The precipitate obtained was filtered and crystallized from ethanol.Crystallization provided pure beta-ketosulfones (1-26).With the intention of high yield, the neutralized filtrate wasevaporated under vacuum and passed through a silica gelgravity column using hexane and ethyl acetate as eluent.The structures of synthetic compounds were deduced byusing 1H-, 13C-NMR, EI-MS, HREI-MS, and elemental analysis.
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