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Structure of 38932-80-8 * 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.
Stage #1: With dihydrogen peroxide In water at 20℃; for 0.5 h; Stage #2: With sulfuric acid; potassium bromide In water at 0℃; for 3 h;
A sample of molybdic acid monohydrate, H2MO04. H20 (0. 16MMOL, 0.029g) was taken in a 250mL glass beaker and 30percent hydrogen peroxide, H2O2 (15. 52MMOL, 1.76mL) was added to it. The mixture was stirred for 30MIN. at room temperature. The solution, which was slightly turbid, was filtered through Whatman No. L filter paper on a glass funnel. The clear filtrate was collected in a 250ML glass beaker and kept in the ice-water bath. Tetrabutylammonium bromide, TBAB (15. 51MMOL, 5G) and potassium bromide, KBr (31. 01MMOL, 3.69g) dissolved in (0. 3M) H2S04 (15. 52MMOL, 51. 70ML) was added to this solution slowly with continuous stirring leading to the formation of a yellow precipitate. The mixture was continued to stir in ice-water bath for another Nlh and then kept standing in ice- water bath for 2h to get an orange yellow compound of Tetrabutylammonium tribromide, TBATB. The compound was separated by filtration under suction using Whatman No. 1 filter paper. It was DRIED IN VACUO over fused CaCl2 and was recrystallized from acetonitrile. Y=7. 23g (96.7percent) MP : 76-77°C. The chemical analyses, IR and conductance of the compound match very well with those reported in literature. Analytical data: The compound analyzed correctly CL6H36NBR3 : Calc. C, 39.86 ; H, 7. 52 ; N, 2. 90 ; Br, 49.71percent. Found. C, 39. 41 ; H, 8. 28 ; N, 2. 78 ; Br, 49. 53. percent.
96.26%
With sulfuric acid; dihydrogen peroxide; potassium bromide In water at 0 - 20℃; for 0.916667 h;
Molybdic acid monohydrate, H2MO04. H20 (0. 16MMOL, 0.029g), potassium bromide, KBr (31. 01MMOL, 3.69g) and tetrabutylammonium bromide, TBAB (15. 51mmol, 5g) were powdered separately, mixed together smoothly and thoroughly. The whole was transferred to a boat kept on ice-water bath and 30percent hydrogen peroxide, H202 (15. 52MMOL, 1.76mL) was added drop wise with continuous grinding for 15 min, followed by drop wise addition of 1 OM H2S04 (15. 5MMOL, 1.55mL) leading to the formation of a yellow colored solution. It was stirred smoothly with glass rod for 10 min and then at room temperature for 30min. An exothermic reaction set in to form orange-yellow crystalline compound of tetrabutylammonium tribromide, TBATB. The compound was dried over fused CaCl2 and extracted with ethyl acetate by dissolving in minimum amount of solvent followed by filtration through Whatman No. 42 filter paper. Aqueous phase, if present, could be separated using anhydrous sodium sulphate. The organic layer was concentrated to get yellow-orange tetrabutylammonium tribromide, TBATB and the latter was recrystallized from acetonitrile. Yield: 7.2g (96.26percent) Mp: 76-77 °C. The chemical analyses, IR and conductance of the compound match very well with those reported in literature. Analytical data: The compound analyzed correctly CL6H36NBR3 : Calc. C, 39.86 ; H, 7.52 ; N, 2.90 ; Br, 49.71percent. Found. C, 39.41 ; H, 8.28 ; N, 2.78 ; Br, 49.53 percent.
96%
With 3-chloro-benzenecarboperoxoic acid; potassium bromide In water for 0.0833333 h;
4. Synthesis of tetrabutyl ammonium tribromide, TBATB: 1 equiv of tetrabutyl ammonium bromide(1 mmol, 0.322 g), 2 equiv of KBr (2 mmol, 0.238 g) and 2 equiv of MCPBA (2 mmol, 0.346 g) weremixed together in 10 mL of water and stirred for ca. 5 min. The orange coloured product formed waswashed with NaHCO3 solution (10 percent solution) for several times to remove unreacted substrate. After thatthe crude product was again washed with water to remove by-products. The compound was dried invacuo and recrystallized with EtOAc; mp: 75oC. Yield: 0.462 g; 96 percent.
96%
Stage #1: With sodium bromate In water at 20℃; for 0.166667 h; Stage #2: With hydrogen bromide In water at 20℃; for 0.5 h;
A mixture of TBAB (38.80 g, 120 mmol), sodium bromate (6.00 g, 40 mmol) and water (300 mL) was stirred at room temperature for 10 min. To this solution was added 48percent Aq. HBr (28 mL) drop wise under stirring and continued for another 30 min at room temperature. An orange colored solid precipitated out, which was filtered, washed with water (2×120 mL) and air-dried at room temperature.Yield: 55.36 g (96percent). mp 74-76°C.
91%
for 0.0833333 h; Green chemistry
An amount of 3.2 g (10 mmol) tetrabutylammonium bromide was added to a solution of 2.4 g (20 mmol) of KBr in 10 mL of 4N H2SO4. To the resulting solution was added 10 mL of 4 percent sodium hypochlorite. The solution was stirred for ca. 5 mins and then the bright orange-yellow colored crystalline TBATB which had separated out was isolated by suction filtration and washed with water (5 mL) three to four times and dried under vacuum over anhydrous CaCl2 to get 4.38 g of TBATB as orange crystals (yield 91percent). Mp: 74 C.
91%
With periodic acid; potassium bromide In neat (no solvent) at 20℃;
General procedure: 1 equiv of tetraalkylammonium bromide (10 mmol), 2 equiv of KBr (20 mmol, 2.38 g)and 2 equiv of H5IO6 (20 mmol, 4.56 g) were mixed together and ground well in a mortar ca. 5-15 minutes. The orange coloured product formed was washed with water for several times to remove by-products. After that the crude product was extracted with ethyl acetate and the organic solvent was dried in vacuo to get pure product. Yield: 82-93 percent (0.3-0.4 g).
Reference：
[1] Patent: WO2004/54962, 2004, A1, . Location in patent: Page 10
[2] Patent: WO2004/54962, 2004, A1, . Location in patent: Page 11-12
[3] Catalysis Communications, 2010, vol. 11, # 11, p. 992 - 995
[4] Synthetic Communications, 2015, vol. 45, # 6, p. 724 - 736
[5] Arkivoc, 2018, vol. 2018, # 7, p. 172 - 185
[6] Chemistry Letters, 2014, vol. 43, # 5, p. 631 - 633
[7] Chemistry Letters, 2014, vol. 43, # 10, p. 1545 - 1547
[8] Synthetic Communications, 2013, vol. 43, # 12, p. 1734 - 1742
[9] Journal of the Chemical Society, Perkin Transactions 2: Physical Organic Chemistry (1972-1999), 1987, p. 39 - 46
[10] Bulletin of the Chemical Society of Japan, 1988, vol. 61, p. 3181 - 3186
[11] Organic Process Research and Development, 2016, vol. 20, # 7, p. 1227 - 1238
[12] Tetrahedron Letters, 2016, vol. 57, # 50, p. 5644 - 5648
[13] Inorganica Chimica Acta, 2018, vol. 469, p. 583 - 587
A sample of molybdic acid monohydrate, H2MO04. H20 (0. 16MMOL, 0.029g) was taken in a 250mL glass beaker and 30% hydrogen peroxide, H2O2 (15. 52MMOL, 1.76mL) was added to it. The mixture was stirred for 30MIN. at room temperature. The solution, which was slightly turbid, was filtered through Whatman No. L filter paper on a glass funnel. The clear filtrate was collected in a 250ML glass beaker and kept in the ice-water bath. Tetrabutylammonium bromide, TBAB (15. 51MMOL, 5G) and potassium bromide, KBr (31. 01MMOL, 3.69g) dissolved in (0. 3M) H2S04 (15. 52MMOL, 51. 70ML) was added to this solution slowly with continuous stirring leading to the formation of a yellow precipitate. The mixture was continued to stir in ice-water bath for another Nlh and then kept standing in ice- water bath for 2h to get an orange yellow compound of Tetrabutylammonium tribromide, TBATB. The compound was separated by filtration under suction using Whatman No. 1 filter paper. It was DRIED IN VACUO over fused CaCl2 and was recrystallized from acetonitrile. Y=7. 23g (96.7%) MP : 76-77C. The chemical analyses, IR and conductance of the compound match very well with those reported in literature. Analytical data: The compound analyzed correctly CL6H36NBR3 : Calc. C, 39.86 ; H, 7. 52 ; N, 2. 90 ; Br, 49.71%. Found. C, 39. 41 ; H, 8. 28 ; N, 2. 78 ; Br, 49. 53. %.
96.26%
With sulfuric acid; dihydrogen peroxide; potassium bromide;molybdic acid; In water; at 0 - 20℃; for 0.916667h;
Molybdic acid monohydrate, H2MO04. H20 (0. 16MMOL, 0.029g), potassium bromide, KBr (31. 01MMOL, 3.69g) and tetrabutylammonium bromide, TBAB (15. 51mmol, 5g) were powdered separately, mixed together smoothly and thoroughly. The whole was transferred to a boat kept on ice-water bath and 30% hydrogen peroxide, H202 (15. 52MMOL, 1.76mL) was added drop wise with continuous grinding for 15 min, followed by drop wise addition of 1 OM H2S04 (15. 5MMOL, 1.55mL) leading to the formation of a yellow colored solution. It was stirred smoothly with glass rod for 10 min and then at room temperature for 30min. An exothermic reaction set in to form orange-yellow crystalline compound of tetrabutylammonium tribromide, TBATB. The compound was dried over fused CaCl2 and extracted with ethyl acetate by dissolving in minimum amount of solvent followed by filtration through Whatman No. 42 filter paper. Aqueous phase, if present, could be separated using anhydrous sodium sulphate. The organic layer was concentrated to get yellow-orange tetrabutylammonium tribromide, TBATB and the latter was recrystallized from acetonitrile. Yield: 7.2g (96.26%) Mp: 76-77 C. The chemical analyses, IR and conductance of the compound match very well with those reported in literature. Analytical data: The compound analyzed correctly CL6H36NBR3 : Calc. C, 39.86 ; H, 7.52 ; N, 2.90 ; Br, 49.71%. Found. C, 39.41 ; H, 8.28 ; N, 2.78 ; Br, 49.53 %.
96%
With 3-chloro-benzenecarboperoxoic acid; potassium bromide; In water; for 0.0833333h;
4. Synthesis of tetrabutyl ammonium tribromide, TBATB: 1 equiv of tetrabutyl ammonium bromide(1 mmol, 0.322 g), 2 equiv of KBr (2 mmol, 0.238 g) and 2 equiv of MCPBA (2 mmol, 0.346 g) weremixed together in 10 mL of water and stirred for ca. 5 min. The orange coloured product formed waswashed with NaHCO3 solution (10 % solution) for several times to remove unreacted substrate. After thatthe crude product was again washed with water to remove by-products. The compound was dried invacuo and recrystallized with EtOAc; mp: 75oC. Yield: 0.462 g; 96 %.
96%
A mixture of TBAB (38.80 g, 120 mmol), sodium bromate (6.00 g, 40 mmol) and water (300 mL) was stirred at room temperature for 10 min. To this solution was added 48% Aq. HBr (28 mL) drop wise under stirring and continued for another 30 min at room temperature. An orange colored solid precipitated out, which was filtered, washed with water (2×120 mL) and air-dried at room temperature.Yield: 55.36 g (96%). mp 74-76C.
91%
With sodium hypochlorite; sulfuric acid; potassium bromide; for 0.0833333h;Green chemistry;
An amount of 3.2 g (10 mmol) tetrabutylammonium bromide was added to a solution of 2.4 g (20 mmol) of KBr in 10 mL of 4N H2SO4. To the resulting solution was added 10 mL of 4 % sodium hypochlorite. The solution was stirred for ca. 5 mins and then the bright orange-yellow colored crystalline TBATB which had separated out was isolated by suction filtration and washed with water (5 mL) three to four times and dried under vacuum over anhydrous CaCl2 to get 4.38 g of TBATB as orange crystals (yield 91%). Mp: 74 C.
91%
With periodic acid; potassium bromide; In neat (no solvent); at 20℃;
General procedure: 1 equiv of tetraalkylammonium bromide (10 mmol), 2 equiv of KBr (20 mmol, 2.38 g)and 2 equiv of H5IO6 (20 mmol, 4.56 g) were mixed together and ground well in a mortar ca. 5-15 minutes. The orange coloured product formed was washed with water for several times to remove by-products. After that the crude product was extracted with ethyl acetate and the organic solvent was dried in vacuo to get pure product. Yield: 82-93 % (0.3-0.4 g).
161 mg (0.5 mmol) of tetrabutylammonium bromide were dissolved in 1 ml of 2M HBr; 2.5 ml of 0.2M solution of Br2 in aqueous 2M HBr (0.5 mmol of bromine) were added. Resulting solution was cooled; orange crystals precipitated.
2-bromo-1-(4-(pentyloxy)phenyl)ethanone 4-Pentyloxyacetophenone (1.3 g, 6.3 mmol) was dissolved in anhydrous CH2Cl2 (20 mL) and anhydrous MeOH (10 mL) under Ar. Tetrabutylammoniumtribromide (3.3 g, 6.9 mmol) was added and the reaction mixture stirred at room temperature for 48 h. Solvent was removed under vacuum and the thick residue passed through a short plug of silica gel eluting with 10% EtOAc in hexane to afford 1.6 g product (91%). 1H NMR (500 MHz, CDCl3): delta 0.96 (t, 3H, J=7.1 Hz), 1.41-1.49 (m, 4H), 1.82-1.87 (m, 2H), 4.04 (t, 2H, J=6.5 Hz), 4.41 (s, 2H), 6.98 (d, 2H, J=7.2 Hz), 7.98 (d, 2 H, J=7.2 Hz).
potassium (trans-1,2-difluorohex-1-en-1-yl)trifluoroborate[ No CAS ]
[ 1361257-64-8 ]
[ 429-42-5 ]
Yield
Reaction Conditions
Operation in experiment
0.32 mmol; 0.7 mmol
In tetrahydrofuran; water; at 20℃; for 0.5h;
K[trans-C4H9CF55CFBF3] (159 mg, 0.70 mmol) was reacted with [Bu4N][Br3] (365 mg, 0.76 mmol) in aq THF (1:1, v/v) (4 mL) as described above and yielded a solution of trans-C4H9CF55CFBr (0.32 mmol) and [Bu4N][BF4] (0.70 mmol) (19F NMR).
Preparation 12 1-(4-Bromo-2-thienyl)-2-(diallylamino)ethanone To 1-(4-bromothiophen-2-yl)ethanone (10 g, 48.8 mmol) in methanol (98 mL) and dichloromethane (163 mL) is added <strong>[38932-80-8]tetra-n-butylammonium tribromide</strong> (28.8 g, 58.5 mmol). The reaction mixture is concentrated under reduced pressure at 50 C. to give a residue which is purified by silica gel chromatography, eluting with dichloromethane to give crude 2-bromo-1-(4-bromo-2-thienyl)ethanone.
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