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[ CAS No. 811-68-7 ]

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Chemical Structure| 811-68-7
Chemical Structure| 811-68-7
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CAS No. :811-68-7 MDL No. :MFCD25563234
Formula : CAgF3S Boiling Point : -
Linear Structure Formula :- InChI Key :N/A
M.W :208.94 g/mol Pubchem ID :-
Synonyms :

Safety of [ 811-68-7 ]

Signal Word:Danger Class:8
Precautionary Statements:P301+P330+P331-P303+P361+P353-P363-P304+P340-P310-P321-P260-P264-P280-P305+P351+P338-P405-P501 UN#:1759
Hazard Statements:H314 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 811-68-7 ]

  • Upstream synthesis route of [ 811-68-7 ]
  • Downstream synthetic route of [ 811-68-7 ]

[ 811-68-7 ] Synthesis Path-Upstream   1~21

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Reference: [1] Advanced Synthesis and Catalysis, 2015, vol. 357, # 16-17, p. 3521 - 3528
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  • [ 75-15-0 ]
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YieldReaction ConditionsOperation in experiment
76% for 18 h; Darkness; Inert atmosphere; Reflux AgF (1 eq, 47.4 mmol, 6 g), CS2 (2.1 eq, 99.3 mmol, 6 mL) in CH3CN(12 mL) were placed in a dark flask under N2 atmosfere and heated to reflux for 18 h. After this time, the mixture was cooled to RT and all the volatile parts were removed under reduced pressure. The remaining black residue was then dissolved in AcOEt, all the insoluble parts werere moved by filtration and the liquid phase was concentrated with the aid of a rotary evaporator. The resulting pale yellow solid was then dissolved in a small amount of CH3CN and 40 mL of Et2O were carefully layered on top of this solution. The mixture was then placed at −15 °Cfor 24 h to produce a needle-shaped white solid that was recovered by filtration and washed with cooled Et2O. The solid was stored at 5 °C with the exclusion of light. Yield: 0.62 g, 76percent. 19F NMR (CD3CN): δ−22.51 (s) ppm.
8 g at 80℃; Inert atmosphere; Glovebox (1) in the glove box 15g into tachiol in the drying reaction bottle, the bottle is covered with the glove box. In a nitrogen atmosphere by adding 80 ml of heavy evaporation of the acetonitrile and 25 ml carbon bisulfide, reflux condensation tube in fast filled 80 °C reflux overnight. Then the carbon bisulfide boil off, then the remaining rotary evaporimeter turns on lathe doesthe nitrile uses b to obtain black solid. Then with ethyl acetate and a black solid dissolve and wash using diatomaceous earth filter, and washing several times. Under lucifugal terms turns on lathe does the filtrate to obtain viscous solid, with 60 after viscous solid dissolving drop second grade nitrile, the 180 ml ethyl ether is slowly added along the bottle wall. This mixed liquid still at room temperature 12 hours later, the -20 ° C for 24 hours. turns on lathe does ethyl ether and to continue to throw a metal luster obtained gray solid tachiol 8 g
Reference: [1] Angewandte Chemie, International Edition, 2014, vol. 53, # 35, p. 9316 - 9320,5[2] Angewandte Chemie, 2014, vol. 126, # 35, p. 9470 - 9474,5
[3] Organic Letters, 2015, vol. 17, # 12, p. 3011 - 3013
[4] Angewandte Chemie - International Edition, 2013, vol. 52, # 12, p. 3457 - 3460[5] Angew. Chem., 2013, vol. 125, # 12, p. 3541 - 3544,4
[6] Catalysis Today, 2018, vol. 308, p. 94 - 101
[7] Journal of the Chemical Society, [8] Journal of the Chemical Society, 1961, p. 2597 - 2599
[9] Journal of the Chemical Society, [10] Journal of the Chemical Society, 1961, p. 2597 - 2599
[11] , Gmelin Handbook: Ag: MVol.B7, 1.20.2.1.1, page 4 - 10,
[12] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
[13] Chemistry - A European Journal, 2014, vol. 20, # 32, p. 9867 - 9870
[14] Angewandte Chemie - International Edition, 2015, vol. 54, # 13, p. 4070 - 4074[15] Angew. Chem., 2015,
[16] European Journal of Organic Chemistry, 2016, vol. 2016, # 6, p. 1091 - 1094
[17] Patent: CN105669503, 2016, A, . Location in patent: Page/Page column 5
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  • [ 14104-20-2 ]
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YieldReaction ConditionsOperation in experiment
89% With triphenylphosphine In acetonitrile at 0 - 50℃; for 12 h; Inert atmosphere Under a nitrogen atmosphere, AgBF4 (19.77 g, 100 mmol) and CF3SO2Na (18.73 g, 120 mmol) were dissolved in anhydrous acetonitrile (400 mL). The reaction solution was cooled to 0°C followed by the addition of Ph3P (62.95 g, 240 mmol). The reaction solution was returned to room temperature. The reaction was heated to 50 ° C for 12 hours. After the reaction, the reaction solution was filtered through celite, and the filtrate was cooled to -20 °C. After sufficient precipitation of crystals, the supernatant was purged to remove most of the triphenylphosphine oxide. The supernatant was removed in vacuo to remove the solvent. The residue was washed thoroughly with ether, vacuum-dried, and the residual solid was recrystallized from tetrahydrofuran and benzene to obtain trifluoromethylthio silver (I) (18.60 g, yield 89percent).
Reference: [1] Patent: CN105017110, 2016, B, . Location in patent: Paragraph 0039; 0040
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  • [ 2923-28-6 ]
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YieldReaction ConditionsOperation in experiment
84% With tri-tert-butyl phosphine In acetonitrile at 0 - 20℃; for 12 h; Inert atmosphere Under a nitrogen atmosphere, AgOTf (25.69 g, 100 mmol) and CF3SO2Na (18.73 g, 120 mmol) was dissolved in anhydrous acetonitrile (400 mL), the reaction solution was cooled to 0°C followed by the addition of tBu3P (50.58 g,250 mmol). The reaction solution was returned to room temperature, and stirred well at room temperature for 12 hours. After the reaction, the reaction solution was filtered through celite, the filtrate was cooled to -20 ° C, and crystals were precipitated. The supernatant was purged to remove most of the tri-tert-butylphosphine oxide. The supernatant was removed in vacuo to remove the solvent. The residue was washed thoroughly with ether, vacuum-dried and the residual solid was recrystallized from tetrahydrofuran and toluene to give the product trifluoromethylthio silver(I) (17.55 g, yield 84percent).
Reference: [1] Patent: CN105017110, 2016, B, . Location in patent: Paragraph 0037; 0038
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YieldReaction ConditionsOperation in experiment
67% With triphenylphosphine In acetonitrile at 0 - 80℃; for 12 h; Inert atmosphere Under nitrogen atmosphere, AgF (12.69 g, 100 mmol) and CF3SO2Na (23.41 g, 150 mmol) was dissolved in anhydrous acetonitrile (400 mL). The reaction solution was cooled to 0 ° C, followed by the addition of Ph3P (83.94 g, 320 mmol). The reaction solution was returned to room temperature and heated to 80°C for 12 hours. After the reaction, the reaction solution was filtered through celite, the filtrate was cooled to -20 °C, and crystals were precipitated. The supernatant was purged to remove most of the triphenylphosphine oxide. The supernatant was removed in vacuo to remove the solvent. The residue was washed thoroughly with ether, vacuum-dried and the residual solid was recrystallized from acetonitrile and ether to give the product trifluoromethylthio silver (I) (14.00 g, yield 67percent).
Reference: [1] Patent: CN105017110, 2016, B, . Location in patent: Paragraph 0033; 0034
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YieldReaction ConditionsOperation in experiment
55% With trimethylphosphane In acetonitrile at 0 - 50℃; for 10 h; Inert atmosphere Under a nitrogen atmosphere, AgCl (14.33 g, 100 mmol) and CF3SO2Na (23.41 g, 150 mmol) was dissolved in anhydrous acetonitrile (500 mL). The reaction solution was cooled to 0 ° C, followed by the addition of Me3P (22.82 g, 300 mmol). The reaction solution was returned to room temperature and heated to 50°C for 10 hours. After the reaction, the reaction solution was filtered through celite, the filtrate was cooled to -20°C, crystals were precipitated, and the supernatant was purged to remove most of the trimethylphosphine oxide. The supernatant was removed in vacuo to remove the solvent. The residue was washed thoroughly with ether, vacuum-dried and the residual solid was recrystallized from acetonitrile and benzene to obtain trifluoromethylthio silver (I) (11.50 g, yield 55percent).
Reference: [1] Patent: CN105017110, 2016, B, . Location in patent: Paragraph 0035; 0036
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YieldReaction ConditionsOperation in experiment
86% at 0 - 20℃; for 12 h; Inert atmosphere Under a nitrogen atmosphere, AgPF6 (25.28 g,100 mmol ) and CF3SO2Na (18.73 g,120 mmol) dissolved in anhydrous acetonitrile (400mL), the reaction solution was cooled to 0°C, followed by the addition of Ph3P (62.95 g, 240 mmol). The reaction solution was returned to room temperature and stirred at room temperature for 12 hours. After the reaction, the reaction solution was filtered through celite, the filtrate was cooled to -20 ° C, and crystals were precipitated. The supernatant was purged to remove most of the triphenylphosphine oxide. The supernatant was removed in vacuo to remove the solvent. The residue was washed thoroughly with ether, vacuum-dried and the residual solid was recrystallized from acetonitrile and toluene to give the product trifluoromethylthio silver (I)(17.97 g, yield 86percent).
Reference: [1] Patent: CN105017110, 2016, B, . Location in patent: Paragraph 0041; 0042
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Reference: [1] Journal of the American Chemical Society, 1959, vol. 81, p. 3575
[2] Journal of the American Chemical Society, 1959, vol. 81, p. 3575
[3] , Gmelin Handbook: Ag: MVol.B7, 1.20.2.1.1, page 4 - 10,
[4] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 15223-20-8 ]
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Reference: [1] Tetrahedron Letters, 2018, vol. 59, # 18, p. 1719 - 1722
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  • [ 15223-20-8 ]
  • [ 455-16-3 ]
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Reference: [1] Tetrahedron Letters, 2018, vol. 59, # 18, p. 1719 - 1722
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  • [ 563-63-3 ]
  • [ 21259-75-6 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1962, p. 1254 - 1260
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 420-32-6 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1960, p. 3516 - 3520
[3] Journal of the Chemical Society, [4] Journal of the Chemical Society, 1962, p. 4361 - 4366
[5] , Gmelin Handbook: F: PerFHalOrg.1, 1.1.1.1, page 1 - 7,
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  • [ 753-94-6 ]
  • [ 506-64-9 ]
  • [ 811-68-7 ]
Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1960, p. 3516 - 3520
[3] , Gmelin Handbook: Ag: MVol.B3, 16.4.1.7.5, page 305 - 307,
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  • [ 563-63-3 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1962, p. 1254 - 1260
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 21259-75-6 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1962, p. 1254 - 1260
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 2966-50-9 ]
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  • [ 811-68-7 ]
Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1962, p. 1254 - 1260
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 21259-75-6 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1962, p. 1254 - 1260
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.11, page 32 - 49,
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  • [ 753-94-6 ]
  • [ 13966-57-9 ]
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1960, p. 3516 - 3520
[3] , Gmelin Handbook: Ag: MVol.B7, 1.20.2.1.1, page 4 - 10,
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  • [ 78910-20-0 ]
  • [ 372-64-5 ]
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Reference: [1] Zeitschrift fuer Naturforschung, [2] Zeitschrift fuer Naturforschung, 1981, vol. 36b, p. 426 - 430
[3] , Gmelin Handbook: F: PerFHalOrg.SVol.3, 6.3.2, page 215 - 245,
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1960, p. 3516 - 3520
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.10, page 27 - 31,
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Reference: [1] Journal of the Chemical Society, [2] Journal of the Chemical Society, 1960, p. 3516 - 3520
[3] , Gmelin Handbook: F: PerFHalOrg.2, 1.1.6.10, page 27 - 31,
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