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type
HazMat fee
Excepted Quantity
Free
Inaccessible (Haz class 6.1), Domestic
USD 41.00
Inaccessible (Haz class 6.1), International
USD 64.00
Accessible (Haz class 3, 4, 5 or 8), Domestic
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Structure of 811-68-7 * Storage: {[proInfo.prStorage]}
Reference：
[1] Advanced Synthesis and Catalysis, 2015, vol. 357, # 16-17, p. 3521 - 3528
2
[ 75-15-0 ]
[ 811-68-7 ]
Yield
Reaction Conditions
Operation 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
3
[ 14104-20-2 ]
[ 2926-29-6 ]
[ 811-68-7 ]
Yield
Reaction Conditions
Operation 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).
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).
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).
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).
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] 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,
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,
12
[ 420-32-6 ]
[ 811-68-7 ]
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,
13
[ 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,
14
[ 563-63-3 ]
[ 21259-75-6 ]
[ 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,
15
[ 21259-75-6 ]
[ 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,
16
[ 2966-50-9 ]
[ 21259-75-6 ]
[ 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,
17
[ 21259-75-6 ]
[ 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,
18
[ 753-94-6 ]
[ 13966-57-9 ]
[ 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.B7, 1.20.2.1.1, page 4 - 10,
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,
21
[ 330660-35-0 ]
[ 753-94-6 ]
[ 11128-24-8 ]
[ 420-32-6 ]
[ 1111-70-2 ]
[ 461-08-5 ]
[ 811-68-7 ]
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,
2-((trifluoromethyl)thio)benzo[d]isothiazol-3(2H)-one 1,1-dioxide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
86%
In acetonitrile; at 20℃; for 0.166667h;
Saccharin (6.0 g) was reacted in methanol (120 ml) at room temperature for 5 minutes with tert-butyl hypochlorite (5 ml) to give the compoundChloro-saccharin 1a (6.0 g, 84%); Chloro-saccharin 1a (3.0 g) was reacted with trifluoromethylthio-silver (3.6 g) in acetonitrile (40 ml) at room temperature for 10 min to give Compound 1 (3.3 g, 86%). Reagent 1 is a white solid at room temperature, soluble in organic solvents such as dichloromethane, chloroform, acetone and acetonitrile.
86%
In acetonitrile; at 20℃; for 0.166667h;
Saccharin (6.0 g of) in methanol (120ml) at room temperature and tert-butyl hypochlorite (5ml) for 5 minutes to give saccharin chloro compound 1a (6.0g, 84%); chloro saccharin 1a (3.0g) and three difluoromethylthio-silver (3.6 g of) in acetonitrile (40ml) and reacted at room temperature for 10 minutes to give compound 1 (3.3g, 86%).Reagent 1 at room temperature a white solid was soluble in methylene chloride, chloroform, acetone, and acetonitrile.N - trifluoromethylthio-saccharin (2 - ((Trifluoromethyl) Thio) of benzo [D] isothiazol-3 (2H) -one1,1-dioxide)
86%
In acetonitrile; at 20℃; for 0.166667h;
Saccharin (6.0 g of) in methanol (120ml) and tert-butyl hypochlorite (5ml) for 5 minutes to give saccharin chloro compound 1a (6.0g, 84%) at room temperature; chloro saccharin 1a (3.0g) and three difluoromethylthio-silver (3.6 g of) the reaction at room temperature in acetonitrile (40ml) 10 minutes to give compound 1 (3.3g, 86%).
86%
In acetonitrile; at 20℃; for 0.166667h;Green chemistry;
Saccharin (6.0 g) was reacted with t-butyl hypochlorite (5 ml) in methanol (120 ml) for 5 minutes at room temperature to give the compound chlorosaccharide 1a (6.0 g, 84%);The chloro saccharin 1a (3.0 g) was reacted with trifluoromethylthio silver (3.6 g) in acetonitrile (40 ml) at room temperature for 10 minutes to give compound II (3.3 g, 86%).The compound II is a white solid at room temperature and is soluble in an organic solvent such as dichloromethane, chloroform, acetone or acetonitrile.
77%
In acetonitrile; at 20℃; for 0.166667h;Inert atmosphere;
<strong>[14070-51-0]N-chlorosaccharin</strong> (1 eq, 1.15 mmol, 250 mg) and AgSCF3 (1.2 eq,1.38 mmol, 288 mg) were dissolved in CH3CN (4 mL) under N2 atmosphere.The mixture was stirred vigorously at room temperature for 10 min. The CH3CN was then drained under reduced pressure. And the residue was extracted with CH2Cl2 (3 mL× 3). The solution wa scombined and the solvent was evaporated under vacuum. The residue was further dried under high vacuum to give compound 2b as a white solid. Yield 251 mg, 77%. 1H NMR (300 MHz, CDCl3): 8.20 (d, 1HJ = 7.5 Hz), 8.08-7.99 (m, 2H), 7.98-7.91 (m, 1H). 19F-NMR (CDCl3): delta -47.73 (s, 3F) ppm. 13C NMR (CDCl3): 158.4,137.9, 136.4, 135.0, 127.8 (q, J = 315 Hz), 126.5, 126.1, 122.0 ppm.
2-bromo-3-trifluoromethylthio-1,4-naphthoquinone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
78%
With dipotassium peroxodisulfate; Cu2(OH)2CO3·H2O; In acetonitrile; at 65℃;Schlenk technique; Inert atmosphere;
General procedure: Procedure A: A 25 mL Schlenk tube equipped with a magnetic stirbar was charged with quinones (0.2 mmol, 1.0 equiv), Cu2(OH)2CO3·H2O(71.7 mg, 0.3 mmol, 1.5 equiv), AgSCF3 (125.3mg, 0.6 mmol, 3.0 equiv), K2S2O8 (162.2mg, 0.6 mmol, 3.0 equiv). The tube was sealed with a septum, evacuated, andbackfilled with nitrogen three times. Then CH3CN (1.0 mL) was addedby a syringe. The mixture was stirred at 65 oCovernight. 5 mL saturated ammonium chloride aqueous solution was added. Theresulting mixture was filtered by Celite, eluted with diethyl ether. Separatedthe layers and the water phase was extracted with diethyl ether. The combinedorganic phase was washed with brine, dried over Na2SO4,filtered, and concentrated under reduced vacuum. The residue was purified withsilica gel column chromatography to provide the pure product.
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