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Product Details of [ 1256808-29-3 ]

CAS No. :1256808-29-3 MDL No. :MFCD18257815
Formula : C7H5BrClNO Boiling Point : -
Linear Structure Formula :- InChI Key :WOJJYMNRQWXZJI-UHFFFAOYSA-N
M.W : 234.48 Pubchem ID :91658963
Synonyms :

Safety of [ 1256808-29-3 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P330-P363-P501 UN#:
Hazard Statements:H302-H312-H332 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 1256808-29-3 ]

* 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.

  • Downstream synthetic route of [ 1256808-29-3 ]

[ 1256808-29-3 ] Synthesis Path-Downstream   1~23

  • 1
  • [ 1256808-29-3 ]
  • [ 1807445-81-3 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 5 steps 1: hydrogen bromide; acetic acid / toluene / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: 18-crown-6 ether; potassium <i>tert</i>-butylate / toluene / 5 h / Reflux 4: methylamine / toluene; water; ethanol / 8 h / 20 °C / Cooling with ice 5: triethylamine / dichloromethane / 1.5 h / 20 °C / Cooling with ice
Multi-step reaction with 5 steps 1: hydrogen bromide; acetic acid; bromine / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: potassium <i>tert</i>-butylate; 18-crown-6 ether / toluene / 5 h / Reflux 4: methylamine / water; toluene; ethanol / 8 h / 20 °C / Cooling with ice 5: triethylamine / dichloromethane / 1.5 h / 20 °C / Cooling with ice
  • 2
  • [ 1256808-29-3 ]
  • [ 1335056-30-8 ]
YieldReaction ConditionsOperation in experiment
89% With hydrogen bromide; bromine; acetic acid In toluene at 20℃; for 18h; 12.1 Step 1: Synthesis of 2-bromo-1- (5-bromo-3-chloropyridin-2-yl) ethanone To a solution of 870 mg of 1- (5-bromo-3-chloropyridin-2-yl) ethanone in 4 ml of toluene was added 7 ml of a 30% by mass solution of hydrobromic acid in acetic acid and then 710 mg of bromine.The reaction was stirred at room temperature for 13 hours.After completion of the stirring, 60 mg of bromine was added to the reaction solution.The reaction was stirred at room temperature for 2 hours.Thereafter, 60 mg of bromine was added to the reaction solution, and after stirring for 3 hours, 50 ml of water was added.Thereafter, the reaction solution is extracted with 50 ml of toluene,It was washed twice with 30 ml of water.The solution was added with 50 ml of ethyl acetate and washed with 50 ml of 2% aqueous sodium bisulfite solution.The solution is dried over anhydrous brine and then dried over anhydrous sodium sulfate,The solvent was distilled off under reduced pressure.The resulting residue is chromatographed on silica gel (ethyl acetate: hex)Purification with a gradient of sun = 0: 10 to 1: 9) gave the desired product 1.03 as a pale yellow solid (yield 89%).
89% Stage #1: 1-(5-bromo-3-chloropyridine-2-yl)ethane-1-on With hydrogen bromide; bromine; acetic acid In toluene at 20℃; for 13h; Stage #2: With bromine In water at 20℃; for 5h; 14.1 Step 1: Synthesis of 2-bromo-1- (5-bromo-3-chloropyridin-2-yl) ethanone In a 4 ml toluene solution of 1- (5-bromo-3-chloropyridin-2-yl) etanone 870 mg, 7 ml of a 30 mass% hydrogen bromide acetic acid solution followed by 710 mg of bromine was added. The reaction was stirred at room temperature for 13 hours. After completion of stirring, 60 mg of bromine was added to the reaction solution. The reaction was stirred at room temperature for 2 hours. Then, 60 mg of bromine was added to the reaction solution, and the mixture was added. After stirring for 3 hours, 50 ml of water was added. Then, the reaction solution was extracted with 50 ml of toluene and washed twice with 30 ml of water. Add 50 ml of ethyl acetate to the solution and 50 ml of 2 mass% sodium bisulfite aqueous solution, The mixture was washed successively with saturated brine, dried over anhydrous sodium sulfate and dehydrated, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel chromatography (ethyl acetate: hexane = 0:10 to 1: 9 gradient) to give the target product 1.03 as a pale yellow solid (yield 89%).
1.7 g With hydrogen bromide; acetic acid In toluene at 20℃; for 23.5h; Cooling with ice; 2.2 preparation of 2-bromo-1- (5-bromo-3-chloropyridin-2-yl)ethanone 5.5ml of 30% hydrogen bromide acetic acid solution was addedto toluene 8ml solution of 1-(5-bromo-3-chloropyridin-2-yl) ethanone 1.60g, andunder ice-cooling and stirring, bromine 1.28g was added dropwise. Afterstirring at room temperature for 18 hours, bromine 0.62g was added, and after2.5 hours, again bromine 0.31 g was added, and then it was stirred continuoslyfor another 3 hours. After completion of the reaction, water 50ml was added tothe reaction mixture and the mixture was extracted with toluene (50 ml × 2).The organic layer was combined and was washed with water 100 ml, and thenwashed with aqueous solution of saturated sodium bisulfite 100 ml, and thendehydrated and dried with saturated brine and then anhydrous sodium sulfate inorder, and the solvent was evaporated under reduced pressure. heptane 20 ml wasadded to the residue and stirred for 30 minutes under ice-cooling, and theprecipitated solid was filtered off to give the desired product 1.7g as whitecrystals.
1.7 g With hydrogen bromide; bromine; acetic acid at 20℃; for 23.5h; Cooling with ice; 6.2 Preparation of 2-bromo-1-(5-bromo-3-chloropyridin-2-yl)ethanone 1- (5-bromo-3-chloro-2-yl) ethanone toluene 8ml solution of 1.60g was added 30% hydrogen bromide acetic acid solution 5.5ml, the stirring under ice-cooling, was added dropwise bromine 1.28 g.Add bromine 0.62g After stirring at room temperature for 18 hours, add an additional 2.5 hours later again bromine 0.31 g, was continued then further stirred for 3 hours.After completion of the reaction, water was added 50ml extracted (50 ml x 2) with toluene to the reaction mixture.After the combined organic layers were washed with water 100 ml, and then saturated aqueous sodium bisulfite 100 ml, saturated saline and then dehydrated and dried and anhydrous sodium sulfate in this order, and the solvent was removed under reduced pressure.Residue stirred for 30 minutes under ice-cooling was added heptane 20 ml, the precipitated solid was filtered off to obtain the desired product 1.7g as white crystals.

  • 3
  • [ 1256808-29-3 ]
  • [ 1807445-78-8 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: hydrogen bromide; acetic acid / toluene / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide
Multi-step reaction with 2 steps 1: hydrogen bromide; acetic acid; bromine / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide
Multi-step reaction with 2 steps 1: acetic acid; bromine; hydrogen bromide / toluene / 18 h / 20 °C 2: N,N-dimethyl-formamide / 5 h / 20 °C
  • 4
  • [ 1256808-29-3 ]
  • [ 1807445-79-9 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1: hydrogen bromide; acetic acid / toluene / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: 18-crown-6 ether; potassium <i>tert</i>-butylate / toluene / 5 h / Reflux
Multi-step reaction with 3 steps 1: hydrogen bromide; acetic acid; bromine / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: potassium <i>tert</i>-butylate; 18-crown-6 ether / toluene / 5 h / Reflux
  • 5
  • [ 1256808-29-3 ]
  • [ 1807445-80-2 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1: hydrogen bromide; acetic acid / toluene / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: 18-crown-6 ether; potassium <i>tert</i>-butylate / toluene / 5 h / Reflux 4: methylamine / toluene; water; ethanol / 8 h / 20 °C / Cooling with ice
Multi-step reaction with 4 steps 1: hydrogen bromide; acetic acid; bromine / 23.5 h / 20 °C / Cooling with ice 2: dimethyl sulfoxide 3: potassium <i>tert</i>-butylate; 18-crown-6 ether / toluene / 5 h / Reflux 4: methylamine / water; toluene; ethanol / 8 h / 20 °C / Cooling with ice
  • 6
  • [ 945557-04-0 ]
  • [ 75-16-1 ]
  • 1-(5-bromo-3-chloropyridine-2-yl)ethane-1-on [ No CAS ]
YieldReaction ConditionsOperation in experiment
44% <strong>[945557-04-0]5-bromo-3-chloropicolinonitrile</strong> (purity 80%)3.84 g are suspended in 40 ml of diethyl ether,It cooled to 0 degreeC.To this suspension, 17 ml of a tetrahydrofuran solution (1 mol / l) of methylmagnesium bromide was dropped.The reaction was stirred at 0 C. for 2.5 hours.After completion of the reaction, the reaction solution was added dropwise to 30 ml of 12 mass% hydrochloric acid cooled to 5 C.After completion of the dropwise addition, the reaction solution was stirred at room temperature for 20 minutes.Thereafter, the reaction solution was extracted with 50 ml of diethyl ether.The organic layer is dried over brine and then over anhydrous sodium sulfate,The solvent was distilled off under reduced pressure.The resulting residue is suspended in 5 ml of hexane,After stirring for 5 minutesThe solid was filtered off and the filtrate was evaporated in vacuo.The resulting residue is purified by silica gel chromatography (ethyl acetate: hexane = 0: 10 to 1: 9 gradient),1.45 g of the desired product was obtained as a white solid (yield 44%).
To 15ml toluene solution of 3.0g of 5-bromo-3-chloropyridin-2-carbonitrile,under ice-cooling and stirring, 3M diethyl ether solution of methyl magnesium bromide4.8ml was dropped, and stirred for 0.5 hours at the same temperature. After thecompletion of the reaction, the reaction mixture was poured under ice-coldstirring into 4N hydrochloric acid 20ml, and extracted with toluene (30mlx2). ).After the organic layer was made together, it was dehydrated and dried in theorder of saturated brine and then anhydrous sodium sulfate, and the solvent wasevaporated under reduced pressure and the desired product 2.7g of crude wasobtained as a brown crystal. This compound without further purification, wasdirectly used in the next step.
To a solution of 3.0 g of <strong>[945557-04-0]5-bromo-3-chloropyridine-2-carbonitrile</strong> in 15 ml of toluene, 4.8 ml of 3 M diethyl ether solution of methyl magnesium bromide was added dropwise with stirring under ice coolingAnd the mixture was stirred at the same temperature for 0.5 hour. After completion of the reaction, the reaction mixture was added to 20 ml of 4N hydrochloric acid by ice cold stirringPoured under stirring, and extracted with toluene (30 ml × 2). The combined organic layer was washed with saturated brine thenAfter drying and drying over anhydrous sodium sulfate in this order, the solvent was distilled off under reduced pressure to obtain 2.7 g of crude target productAs brown crystals. This product was used for the next step without further purification.
  • 7
  • [ 1256808-29-3 ]
  • [ 2083642-19-5 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1.1: sodium hydride / dimethyl sulfoxide / 0.5 h / Cooling with ice 1.2: 15 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide / 6 h / 100 °C
Multi-step reaction with 2 steps 1.1: sodium hydride / dimethyl sulfoxide; paraffin oil / 0.5 h / 0 °C 1.2: 15 h / 0 - 20 °C 2.1: dimethyl sulfoxide / 6 h / 100 °C
  • 8
  • [ 1256808-29-3 ]
  • [ 2083642-20-8 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1.1: sodium hydride / dimethyl sulfoxide / 0.5 h / Cooling with ice 1.2: 15 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 50 °C
Multi-step reaction with 3 steps 1.1: sodium hydride / dimethyl sulfoxide; paraffin oil / 0.5 h / 0 °C 1.2: 15 h / 0 - 20 °C 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 0 - 50 °C
  • 9
  • [ 1256808-29-3 ]
  • [ 2083592-34-9 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1.1: sodium hydride / dimethyl sulfoxide / 0.5 h / Cooling with ice 1.2: 15 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 50 °C 4.1: bis-triphenylphosphine-palladium(II) chloride; triethylamine; copper(l) iodide / N,N-dimethyl-formamide / 5 h / 20 °C / Inert atmosphere
  • 10
  • [ 1256808-29-3 ]
  • [ 2083592-30-5 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 5 steps 1.1: sodium hydride / dimethyl sulfoxide / 0.5 h / Cooling with ice 1.2: 15 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 50 °C 4.1: bis-triphenylphosphine-palladium(II) chloride; triethylamine; copper(l) iodide / N,N-dimethyl-formamide / 5 h / 20 °C / Inert atmosphere 5.1: hydrazine hydrate / ethanol / 1 h / 60 °C
  • 11
  • [ 1256808-29-3 ]
  • [ 2083641-98-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 6 steps 1.1: sodium hydride / dimethyl sulfoxide / 0.5 h / Cooling with ice 1.2: 15 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 50 °C 4.1: bis-triphenylphosphine-palladium(II) chloride; triethylamine; copper(l) iodide / N,N-dimethyl-formamide / 5 h / 20 °C / Inert atmosphere 5.1: hydrazine hydrate / ethanol / 1 h / 60 °C 6.1: triethylamine; dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride / dichloromethane / 16 h / 20 °C
  • 12
  • [ 1256808-29-3 ]
  • [ 1774-47-6 ]
  • [ 2083642-18-4 ]
YieldReaction ConditionsOperation in experiment
5.7 g Stage #1: trimethylsulfoxonium iodide With sodium hydride In dimethyl sulfoxide for 0.5h; Cooling with ice; Stage #2: 1-(5-bromo-3-chloropyridine-2-yl)ethane-1-on In dimethyl sulfoxide at 20℃; for 15h; Cooling with ice; 8-1 Preparation of 5-bromo-3-chloro-2-(2-methyloxiran-2-yl)pyridine Trimethylsulfoxonium iodide 5.2 gIn 15 ml of dimethylsulfoxide,Under ice-cooling and stirring,1.1 g of 55% oily sodium hydride was added,And the mixture was stirred at the same temperature for 30 minutes.Then,The reaction mixture was stirred under ice-cooling1- (5-Bromo-3-chloropyridin-2-yl) ethan-1-one 5.0 gIn 10 ml of dimethylsulfoxide,After completion of the dropwise addition,Stirring was continued for further 15 hours at room temperature.After completion of the reaction,Water (20 ml) was added to the reaction mixture, followed by extraction with ethyl acetate (30 ml × 1).The organic layer was washed with water (30 ml × 1)Dehydrated and dried in the order of saturated saline and then anhydrous sodium sulfate,The solvent was distilled off under reduced pressure.The residue was purified by silica gel column chromatography eluting with ethyl acetate-hexane (0: 10 to 3: 7 gradient)5.7 g of the objective compound was obtained as a brown resinous material.
  • 13
  • [ 1256808-29-3 ]
  • [ 1807444-20-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 6 steps 1.1: hydrogen bromide; acetic acid; bromine / 23.5 h / 20 °C / Cooling with ice 2.1: dimethyl sulfoxide 3.1: potassium <i>tert</i>-butylate; 18-crown-6 ether / toluene / 5 h / Reflux 4.1: methylamine / water; toluene; ethanol / 8 h / 20 °C / Cooling with ice 5.1: triethylamine / dichloromethane / 1.5 h / 20 °C / Cooling with ice 6.1: zinc dibromide / tetrahydrofuran / 0.17 h / Inert atmosphere; Cooling with ice 6.2: 2.5 h / 20 °C / Inert atmosphere
  • 14
  • [ 1256808-29-3 ]
  • [ 1774-47-6 ]
  • [ CAS Unavailable ]
YieldReaction ConditionsOperation in experiment
5.7 g Stage #1: trimethylsulfoxonium iodide With sodium hydride In dimethyl sulfoxide; paraffin oil at 0℃; for 0.5h; Stage #2: 1-(5-bromo-3-chloropyridine-2-yl)ethane-1-on In dimethyl sulfoxide; paraffin oil at 0 - 20℃; for 15h; 1.1B.1 Step 1 : Preparation of 5-bromo-3-chloro-2-(2-methyloxlane-2-yl)pyridine To a stirred solution of trimethylsulfoxonium iodide (5.2g) in DMSO (15ml) at 0°C was added sodium hydride (55 wt%, dispersion in Paraffin Liquid) (1.1g). After stirring at same temperature for 0.5h, the reaction mixture was added dropwise to a stirred solution of 1-(5-bromo-3-chloropyridine-2-yl)ethane-1-on (5.0g) in DMSO (10ml) at 0°C, which was stirred at room temperature for additional 15h. After the completion of the reaction, the reaction mixture was added with water (20ml) and extracted with ethyl acetate (30ml x 1 ). The organic extract was washed with water (30ml x 1 ) and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to provide a residue. The residue was purified by column chromatography on silica gel eluted with ethyl acetate-hexane (volume ratio 0: 10 to 3:7 gradient composition) to afford the title compound as a brown resin (5.7g).NMR (CDCIs, Me4Si, 300MHz) 58.66 (d, J=1 8Hz, 1 H), 8.36 (d, J=1.8Hz, 1 H), 3.03 (d, J=5.2Hz, 1 H), 2.92 (d, J=5.2Hz, 1 H), 1 .58 (s, 3H).
  • 15
  • [ 1256808-29-3 ]
  • [ 2171089-74-8 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1.1: sodium hydride / dimethyl sulfoxide; paraffin oil / 0.5 h / 0 °C 1.2: 15 h / 0 - 20 °C 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 0 - 50 °C 4.1: triethylamine; copper(l) iodide; bis(triphenylphosphine)palladium(II) chloride / N,N-dimethyl-formamide / 5 h / 60 °C / Inert atmosphere
  • 16
  • [ 1256808-29-3 ]
  • [ 2171086-95-4 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 5 steps 1.1: sodium hydride / dimethyl sulfoxide; paraffin oil / 0.5 h / 0 °C 1.2: 15 h / 0 - 20 °C 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 0 - 50 °C 4.1: triethylamine; copper(l) iodide; bis(triphenylphosphine)palladium(II) chloride / N,N-dimethyl-formamide / 5 h / 60 °C / Inert atmosphere 5.1: hydrazine hydrate / ethanol / 5 h / 80 °C
  • 17
  • [ 1256808-29-3 ]
  • [ 2171083-48-8 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 6 steps 1.1: sodium hydride / dimethyl sulfoxide; paraffin oil / 0.5 h / 0 °C 1.2: 15 h / 0 - 20 °C 2.1: dimethyl sulfoxide / 6 h / 100 °C 3.1: (bis-(2-methoxyethyl)amino)sulfur trufluoride / dichloromethane / 12 h / 0 - 50 °C 4.1: triethylamine; copper(l) iodide; bis(triphenylphosphine)palladium(II) chloride / N,N-dimethyl-formamide / 5 h / 60 °C / Inert atmosphere 5.1: hydrazine hydrate / ethanol / 5 h / 80 °C 6.1: triethylamine / dichloromethane / 1 h / 0 - 20 °C
  • 18
  • [ 69739-34-0 ]
  • [ 1256808-29-3 ]
  • [ 2661483-23-2 ]
YieldReaction ConditionsOperation in experiment
84% With triethylamine In dichloromethane at 25℃; for 6h; 67.2 Step 2: 5-bromo-2-(1-((tert-butyldimethylsilyl)oxy)vinyl)-3-chloropyridine To a stirred solution of 1-(5-bromo-3-chloropyridin-2-yl)ethan-1-one (2.0 g, 8.4 mmol) indichloromethane (100 mL) were added TEA (2.5 g, 25.3 mmol) and tert-Butyldimethylsilyl trifluoromethanesulfonate (2.9 g, 10.9 mmol). The mixture was stirred at 25 °C for 6 h. The resulting mixture was diluted with water (100 mL). The resulting mixture was extracted with dichloromethane (3 x 200 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was purified by column chromatography on silica gel using 90% petroleum ether and 10% ethyl acetate as eluent to afford 5-bromo-2-(1-((tert- butyldimethylsilyl)oxy)vinyl)-3-chloropyridine (2.5 g, 84% yield) as a yellow solid.1H NMR (300 MHz, Chloroform-d) δ 8.52 (d, J = 2.1 Hz, 1H), 7.87 (d, J = 2.1 Hz, 1H), 4.82 (d, J = 1.8 Hz, 1H), 4.77 (d, J = 1.8 Hz, 1H), 0.92 (s, 9H), 0.17 (s, 6H). LC-MS: m/z 348 [M+H]+.
  • 19
  • [ 1256808-29-3 ]
  • [ 2661483-24-3 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: triethylamine / dichloromethane / 6 h / 25 °C 2: diethylzinc / hexane; diethyl ether / 2 h / 0 - 40 °C
  • 20
  • [ 1256808-29-3 ]
  • [ 2661483-25-4 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1: triethylamine / dichloromethane / 6 h / 25 °C 2: diethylzinc / hexane; diethyl ether / 2 h / 0 - 40 °C 3: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 110 °C / Inert atmosphere
  • 21
  • [ 1256808-29-3 ]
  • [ 2661483-26-5 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 4 steps 1: triethylamine / dichloromethane / 6 h / 25 °C 2: diethylzinc / hexane; diethyl ether / 2 h / 0 - 40 °C 3: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 110 °C / Inert atmosphere 4: sodium acetate; hydroxylamine hydrochloride / methanol / 16 h / 25 °C
  • 22
  • [ 1256808-29-3 ]
  • [ 2661483-27-6 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 5 steps 1.1: triethylamine / dichloromethane / 6 h / 25 °C 2.1: diethylzinc / hexane; diethyl ether / 2 h / 0 - 40 °C 3.1: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 110 °C / Inert atmosphere 4.1: sodium acetate; hydroxylamine hydrochloride / methanol / 16 h / 25 °C 5.1: triethylamine / tetrahydrofuran / 0.5 h / 0 - 25 °C 5.2: 2 h / 40 °C
  • 23
  • [ 1256808-29-3 ]
  • [ 2661481-69-0 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 6 steps 1.1: triethylamine / dichloromethane / 6 h / 25 °C 2.1: diethylzinc / hexane; diethyl ether / 2 h / 0 - 40 °C 3.1: tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 110 °C / Inert atmosphere 4.1: sodium acetate; hydroxylamine hydrochloride / methanol / 16 h / 25 °C 5.1: triethylamine / tetrahydrofuran / 0.5 h / 0 - 25 °C 5.2: 2 h / 40 °C 6.1: tetrabutyl ammonium fluoride / tetrahydrofuran / 48 h / 25 °C
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