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[ CAS No. 6012-97-1 ] {[proInfo.proName]}

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Product Details of [ 6012-97-1 ]

CAS No. :6012-97-1 MDL No. :MFCD00005422
Formula : C4Cl4S Boiling Point : -
Linear Structure Formula :- InChI Key :WZXXZHONLFRKGG-UHFFFAOYSA-N
M.W : 221.92 Pubchem ID :22344
Synonyms :

Safety of [ 6012-97-1 ]

Signal Word:Danger Class:6.1
Precautionary Statements:P261-P280-P301+P310-P311 UN#:2811
Hazard Statements:H301+H311+H331 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 6012-97-1 ]

* 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 [ 6012-97-1 ]

[ 6012-97-1 ] Synthesis Path-Downstream   1~83

  • 1
  • [ 188290-36-0 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
33% With benzyltrimethylazanium tetrachloro-λ3-iodanuide In acetic acid at 70℃; for 24h;
With chlorine anschliessend Erhitzen auf 200grad;
  • 2
  • [ 1003-09-4 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
With ethanol; chlorine; potassium carbonate
  • 3
  • [ 1003-09-4 ]
  • [ 6012-97-1 ]
  • [ 17249-77-3 ]
YieldReaction ConditionsOperation in experiment
Einleiten von Chlor;
  • 4
  • [ 3141-27-3 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
With ethanol; chlorine; potassium carbonate
  • 5
  • [ 18614-15-8 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
at 215℃;
  • 6
  • [ 6012-97-1 ]
  • [ 857588-15-9 ]
  • 8,11-dimethyl-dinaphtho[1,2,3-<i>de</i>;1',2',3'-<i>d'e'</i>]thieno[3,2-<i>b</i>;4,5-<i>b'</i>] dichromium ene-5,14-dione [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium acetate; 1,2,3-trichlorobenzene
  • 7
  • [ 6012-97-1 ]
  • [ 75-07-0 ]
  • [ 119255-52-6 ]
YieldReaction ConditionsOperation in experiment
With ethyl bromide; diethyl ether; magnesium
With n-butyllithium; diethyl ether
  • 8
  • [ 6012-97-1 ]
  • [ 67-64-1 ]
  • [ 148273-32-9 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium; diethyl ether
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 9
  • [ 6012-97-1 ]
  • [ 17249-78-4 ]
YieldReaction ConditionsOperation in experiment
77% With n-butyllithium In diethyl ether 1 Preparation of 2,3,4-Trichlorothiophen PREPARATION 1 Preparation of 2,3,4-Trichlorothiophen A solution of n-butyl lithium (48.3 ml. of 1.55M, 75 mmole) was added dropwise to a stirred solution of tetrachlorothiophen (16.65 g., 75 mmole) in diethyl ether (150 ml.) at -78° C. After the addition was complete the mixture was stirred at -78° C. for 1 hour and was then diluted with acetic acid (6 ml.) in diethyl ether (25 ml.). The mixture was allowed to come to room temperature and the organic phase was separated. The aqueous layer was extracted with diethyl ether and the combined organic layers were dried (MgSO4) and evaporated and residue distilled to give the desired product (10.9 g., 77%), b.p. 88°-91° at 16 mm Hg.
With methyl bromide; diethyl ether; magnesium anschliessend hydrolysieren;
  • 10
  • [ 6012-97-1 ]
  • [ 18614-14-7 ]
YieldReaction ConditionsOperation in experiment
With tetrachloromethane; iodine; chlorine
  • 11
  • [ 6012-97-1 ]
  • [ 26020-48-4 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium; diethyl ether Behandeln der Reaktionsloesung mit Kohlendioxid;
With diethyl ether; magnesium; methyl iodide Behandeln der Reaktionsloesung mit Kohlendioxid;
  • 13
  • [ 87-68-3 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
56% With sulfur at 210 - 225℃;
With sulfur Entfernen des entstehenden Dischwefeldichlorids;
  • 14
  • [ 6012-97-1 ]
  • [ 344-04-7 ]
  • [ 22096-15-7 ]
YieldReaction ConditionsOperation in experiment
(i) Mg, Et2O, (ii) /BRN= 118374/, cyclohexane; Multistep reaction;
  • 15
  • [ 6012-97-1 ]
  • [ 2418-22-6 ]
  • [ 2418-21-5 ]
YieldReaction ConditionsOperation in experiment
With antimonypentachloride; antimony pentafluoride Heating;
  • 16
  • [ 6012-97-1 ]
  • [ 2418-21-5 ]
YieldReaction ConditionsOperation in experiment
With antimonypentachloride; antimony pentafluoride Heating;
  • 17
  • [ 6012-97-1 ]
  • [ 434-41-3 ]
YieldReaction ConditionsOperation in experiment
With antimonypentachloride; antimony pentafluoride Heating;
  • 18
  • [ 17249-78-4 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
91.2% With chlorine for 3h;
  • 19
  • [ 14371-10-9 ]
  • [ 6012-97-1 ]
  • [ 148273-31-8 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 20
  • [ 6012-97-1 ]
  • [ 50-00-0 ]
  • [ 68639-16-7 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 21
  • [ 6012-97-1 ]
  • [ 123-73-9 ]
  • 4-(3,4,5-trichloro-2-thienyl)-3-butene-2-ol [ No CAS ]
  • 1-(3,4,5-trichloro-2-thienyl)-2-buten-1-ol [ No CAS ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 23
  • [ 7270-63-5 ]
  • [ 6012-97-1 ]
  • 2,3,4,5-tetrachlorotiophenium (4',4'-dimethyl-3',5'-dioxane-2',6'-dione) 1'-S,C-ylide [ No CAS ]
YieldReaction ConditionsOperation in experiment
37% In 1,2-dichloro-ethane at 50 - 80℃; for 96h;
  • 24
  • [ 6012-97-1 ]
  • [ 29397-21-5 ]
  • [ 123004-68-2 ]
YieldReaction ConditionsOperation in experiment
11% at 10℃; for 144h;
  • 25
  • [ 6012-97-1 ]
  • [ 817-87-8 ]
  • [ 90454-50-5 ]
YieldReaction ConditionsOperation in experiment
49% at 130℃; for 0.666667h;
44% at 130℃; for 0.666667h;
  • 26
  • [ 6012-97-1 ]
  • [ 2009-97-4 ]
  • C-acetyl-C-ethoxycarbonyl-(2,3,4,5-tetrachloro-1-thiophenio)-methylide [ No CAS ]
YieldReaction ConditionsOperation in experiment
83% With dirhodium tetraacetate for 72h; Ambient temperature;
  • 27
  • [ 6012-97-1 ]
  • [ 6773-29-1 ]
  • [ 106550-55-4 ]
YieldReaction ConditionsOperation in experiment
75% With dirhodium tetraacetate for 24h; Ambient temperature;
  • 28
  • [ 6012-97-1 ]
  • [ 13298-76-5 ]
  • [ 117112-08-0 ]
YieldReaction ConditionsOperation in experiment
75% for 67h; Ambient temperature;
Ambient temperature;
  • 29
  • [ 6012-97-1 ]
  • [ 17667-39-9 ]
  • [ 59-49-4 ]
  • [ 90454-51-6 ]
YieldReaction ConditionsOperation in experiment
1: 48% 2: 23% at 145℃; for 0.666667h;
  • 30
  • [ 6012-97-1 ]
  • [ 17667-39-9 ]
  • [ 90454-51-6 ]
YieldReaction ConditionsOperation in experiment
23% at 145℃;
  • 31
  • [ 6012-97-1 ]
  • [ 14073-97-3 ]
  • [ 118012-97-8 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) ether, -78 deg C, 30 min, 2.) ether, -78 deg C to room t., 1 h; Yield given. Multistep reaction;
  • 32
  • [ 6012-97-1 ]
  • [ 1807-68-7 ]
  • 2,3,4,5-tetrachlorotiophenium (4',4'-dimethylcyclohexane-2',6'-dione) 1'-S,C-ylide [ No CAS ]
YieldReaction ConditionsOperation in experiment
67% for 168h; Ambient temperature;
Ambient temperature;
  • 33
  • [ 6012-97-1 ]
  • [ 1807-68-7 ]
  • [ 117112-05-7 ]
YieldReaction ConditionsOperation in experiment
93% at 50℃; for 28h;
  • 34
  • [ 6012-97-1 ]
  • [ 3422-06-8 ]
  • [ 113318-90-4 ]
YieldReaction ConditionsOperation in experiment
16% at 130℃; for 0.5h;
  • 35
  • [ 6012-97-1 ]
  • [ 13298-73-2 ]
  • 2,3,4,5-tetrachlorothiophenium C-(ethoxycarbonyl)-C-<(N-tosylamino)carbonyl>methylide [ No CAS ]
YieldReaction ConditionsOperation in experiment
88% at 75℃; for 16h;
  • 36
  • [ 6012-97-1 ]
  • [ 555-16-8 ]
  • 3,4,5-trichloro-2-thienyl(p-nitrophenyl)methanol [ No CAS ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 37
  • [ 6012-97-1 ]
  • α-acetyl-α-p-tosyldiazomethane [ No CAS ]
  • [ 117130-95-7 ]
YieldReaction ConditionsOperation in experiment
26% In 1,2-dichloro-ethane for 336h; Ambient temperature;
  • 38
  • [ 6012-97-1 ]
  • [ 108197-11-1 ]
  • 2,3,4,5-tetrachlorotiophenium C-(ethoxycarbonyl)-C-(benzylsulfonyl)methylide [ No CAS ]
YieldReaction ConditionsOperation in experiment
53% In 1,2-dichloro-ethane for 120h; Ambient temperature;
  • 39
  • [ 6012-97-1 ]
  • [ 100-52-7 ]
  • [ 148273-27-2 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) Et2O, hexane, from -78 deg C to -20 deg C, 15 min, 2.) Et2O, RT, 15 min; Yield given. Multistep reaction;
  • 40
  • [ 6012-97-1 ]
  • [ 160890-91-5 ]
  • [ 118013-07-3 ]
YieldReaction ConditionsOperation in experiment
29% at 135℃;
  • 41
  • [ 6012-97-1 ]
  • [ 118013-06-2 ]
  • [ 118013-08-4 ]
YieldReaction ConditionsOperation in experiment
48% at 135℃;
  • 42
  • [ 6012-97-1 ]
  • cis-2-methylcyclohexyl azidoformate [ No CAS ]
  • (2,3,4,5-Tetrachloro-1λ4-thiophen-1-ylidene)-carbamic acid (1R,2S)-2-methyl-cyclohexyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
17% at 130℃; for 1h;
  • 43
  • [ 6012-97-1 ]
  • trans-2-methylcyclohexyl azidoformate [ No CAS ]
  • (2,3,4,5-Tetrachloro-1λ4-thiophen-1-ylidene)-carbamic acid (1R,2R)-2-methyl-cyclohexyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
15% at 130℃; for 1.5h;
  • 44
  • [ 6012-97-1 ]
  • [ 1516-56-9 ]
  • [ 106550-54-3 ]
YieldReaction ConditionsOperation in experiment
16% at 136℃; for 0.666667h;
  • 45
  • [ 6012-97-1 ]
  • [ 72448-17-0 ]
  • [ 72524-62-0 ]
YieldReaction ConditionsOperation in experiment
50% With 3-chloro-benzenecarboperoxoic acid In 1,2-dichloro-ethane for 48h; Heating;
1.1% With 3-chloro-benzenecarboperoxoic acid In 1,2-dichloro-ethane for 72h; Heating;
  • 46
  • [ 6012-97-1 ]
  • [ 73308-57-3 ]
YieldReaction ConditionsOperation in experiment
With chromium(VI) oxide In acetic acid Heating; Yield given;
  • 47
  • [ 6012-97-1 ]
  • [ 78665-33-5 ]
  • C4Br2Cl2Mg2S [ No CAS ]
YieldReaction ConditionsOperation in experiment
1: 12% 2: 66% With ethylmagnesium bromide In tetrahydrofuran
  • 48
  • [ 127-18-4 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
74 % Turnov. With hydrogen sulfide at 450℃; for 15.5h;
  • 49
  • [ 127-18-4 ]
  • [ 6012-97-1 ]
  • [ 87-68-3 ]
YieldReaction ConditionsOperation in experiment
1: 38.5% 2: 27.9% With hydrogen sulfide at 550℃; for 4h; other temp., (600 deg C); other reaction time ( 9 h);
  • 50
  • [ 110-82-7 ]
  • [ 90454-50-5 ]
  • [ 6012-97-1 ]
  • [ 1541-19-1 ]
YieldReaction ConditionsOperation in experiment
1: 85% 2: 81% Irradiation;
  • 51
  • [ 61351-34-6 ]
  • [ 6012-97-1 ]
  • [ 118888-36-1 ]
YieldReaction ConditionsOperation in experiment
1: 52% 2: 4% With sulfur at 195 - 200℃; for 5h;
  • 52
  • [ 498-66-8 ]
  • [ 106550-55-4 ]
  • [ 6012-97-1 ]
  • [ 1733-15-9 ]
  • (1S,4R,4aR,8aS)-5,6,7,8-Tetrachloro-1,2,3,4,4a,8a-hexahydro-1,4-methano-naphthalene [ No CAS ]
YieldReaction ConditionsOperation in experiment
1: 18% 2: 43% 3: 108 % In acetonitrile for 64h; Heating;
  • 53
  • [ 90454-50-5 ]
  • [ 6012-97-1 ]
  • [ 1124-54-5 ]
YieldReaction ConditionsOperation in experiment
1: 81% 2: 85% In cyclohexane for 1h; Irradiation;
  • 54
  • [ 90454-50-5 ]
  • [ 6012-97-1 ]
  • [ 51-79-6 ]
YieldReaction ConditionsOperation in experiment
1: 61% 2: 68% With hydrogen In tetrahydrofuran for 4h;
68% With hydrogen
  • 55
  • [ 106550-55-4 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
79% With 3-chloro-benzenecarboperoxoic acid In 1,2-dichloro-ethane for 0.0833333h; Heating;
  • 56
  • [ 90454-51-6 ]
  • [ 6012-97-1 ]
  • [ 59-49-4 ]
YieldReaction ConditionsOperation in experiment
1: 46% 2: 48% In dichloromethane for 2h; Irradiation;
  • 57
  • [ 6012-97-1 ]
  • [ 2009-97-4 ]
  • [ 117112-07-9 ]
YieldReaction ConditionsOperation in experiment
Ambient temperature;
  • 58
  • [ 6012-97-1 ]
  • [ 2725-60-2 ]
  • [ 117130-95-7 ]
YieldReaction ConditionsOperation in experiment
Ambient temperature;
  • 59
  • [ 6012-97-1 ]
  • [ 79-22-1 ]
  • [ 81730-18-9 ]
YieldReaction ConditionsOperation in experiment
With n-butyllithium 1.) ether, cyclohexane, -78 deg C, 1 h, 2.) ether, cyclohexane, -78 deg C, 30 min; Yield given. Multistep reaction;
  • 60
  • [ 188290-36-0 ]
  • [ 6012-97-1 ]
  • [ 17249-77-3 ]
YieldReaction ConditionsOperation in experiment
1: 11% 2: 59% With chlorine; iron(III) chloride In tetrachloromethane at 30℃; for 10h;
1: 59% 2: 11% With chlorine; iron(III) chloride In tetrachloromethane at 30℃; for 9h;
  • 61
  • [ 3172-52-9 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
Rk. mit AgF2 (0grad) -> 2,2,5,5-Tetrafluor-3,4-dichlor-thiolen-3;
Rk. mit n-Butyl-Li;
Rk. mit Mg/Ethylenbromid;
Rk. mit LiAlH4 -> (I);
Rk.m.Te, Rongalit, H2O/MeOH/NaOH, Δ -> 2,3,4-Trichlor-thiophen, geringe Mengen 3,4-Dichlorthiophen;
Rk.m.Na-tellurid, wss.MeOH, Δ -> 3,4-Dichlor-thiophen (Hauptprodukt), 2,3,4-Trichlorthiophen;
Rk.m.konz.HNO3 -> 86percent Dichlormaleinsaeure-thioanhydrid, 14percent Dichlormaleinsaeureanhydrid;

YieldReaction ConditionsOperation in experiment
2,5-Dibrom-thiophen, Cl2 (sd. CCl4);
Octachlorthiolan (2), HF/SbCl5;
Thiophen, Chlor;
Hexachlorbutadien, Schwefel;
Hexachlorthiolen, Schwefel (4h,200grad) (Meth.A);
Hexachlorthiolen, S2Cl2 (8h,180-200grad);
Hexachlorthiolen, Cu-Staub (unter Rueckfluss 8h halten);
/BRN= 383664/, CuCl;
Tetrahydrothiophen, Chlorierung-Dehydrohalogenierung;

  • 64
  • [ 87-68-3 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
62% With sulfur at 200 - 225℃; for 29h;
  • 65
  • [ 87-68-3 ]
  • [ 6012-97-1 ]
YieldReaction ConditionsOperation in experiment
at 205 - 240℃;
  • 66
  • [ 6012-97-1 ]
  • 2-hydroxy-3,4,5-trichlorothiophene [ No CAS ]
YieldReaction ConditionsOperation in experiment
74% Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In hexane at -40℃; Stage #2: With boric acid tributyl ester In diethyl ether; hexane at -78℃; for 3h; Stage #3: With dihydrogen peroxide In diethyl ether heating; Further stages.;
  • 67
  • [ 6012-97-1 ]
  • [ 31557-17-2 ]
YieldReaction ConditionsOperation in experiment
With isopropylmagnesium bromide In tetrahydrofuran at 25℃; for 2h;
  • 69
  • [ 6012-97-1 ]
  • [ 5876-51-7 ]
  • 5-(3,4,5-trichloro-2-thienyl)-1,3-benzodioxole [ No CAS ]
  • 70
  • [ 6012-97-1 ]
  • tropine [ No CAS ]
  • endo-3-(3,4,5-trichlorothiophen-2-yloxy)-8-methyl-8-azabicyclo[3.2.1]octane [ No CAS ]
YieldReaction ConditionsOperation in experiment
33% With potassium <i>tert</i>-butylate In DMF (N,N-dimethyl-formamide) at 100℃; for 15h; A Method A; ENDO-3- (3, 4, 5-TRICHLOROTHIOPEN-2-YLOXY)-S-MOTHYL-B-AZABICYCLO [3. 2.1] octane fumaric acid salt A mixture of tetrachlorothiophene (5.48 g, 24.69 mmol), tropine (endo-8-methyl-8- azabicyclo [3.2. 1] octan-3-ol) (3.48 g, 24.69 MMOL), POTASSIUM-TERI-BUTOXIDE (4.16 g, 37.04 mmol), 18-crown-6-ether (6.53 g, 24.69 mmol) and DMF (50 ML) was stirred at 100C for 15 h. Aqueous hydrochloric acid (50 ML, 4 M) was added to the mixture. The mixture was washed with diethyl ether (2 x 100 ML). Aqueous sodium hydroxide (100 ML, 4 M) was added. The mixture was extracted with ethyl acetate (3 x 100 ML). The organic phase was washed with aqueous sodium chloride (3 x 50 ML). Yield 2.65 G (33%). The corresponding salt was obtained by addition of a diethyl ether and methanol mixture (9: 1) saturated with fumaric acid. Mp 200.4-206. 4C.
  • 71
  • [ 6012-97-1 ]
  • [ 24622-15-9 ]
YieldReaction ConditionsOperation in experiment
Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In hexanes; diethyl ether at -45℃; for 0.5h; Stage #2: With sulfur dioxide In hexanes; diethyl ether at -78 - 20℃; for 2h; Stage #3: With N-chloro-succinimide In water; acetic acid at 0 - 20℃; for 1h; 1.a Example 1;3,4,5-Trichloro-A/-(3-methoxypyrazin-2-yl)thiophene-2-sulphonamide;a) 3,4,5-Trichlorothiophene-2-sulphonyl chloride Tetrachlorothiophene (lO.Og) in dry ether (100 ml) was treated with n-butyl lithium (1.3 Msolution in hexanes, 35 ml) at -45C and stirred for 30 minutes, under an dry nitrogenatmosphere. The solution was cooled to -78C and treated with a saturated solution ofsulphur dioxide in ether (20 ml). The mixture was stirred at -78C for 30 minutes, andthen allowed to warm to room temperature over 90 minutes. The resulting suspension wasconcentrated under reduced pressure and the residue was redissolved in acetic acid (35 ml)and water (35 ml). The solution resulting was treated with JV-chlorosuccinimide (6.0 g)portionwise at 0C, and then stirred at room temperature for 1 hour. The suspended solidwas removed by filtration and dried in air to afford the subtitled compound as an orangepowder (9.7 g).m/e 284/286/288 (M+), 100%.MP 56 C.
  • 72
  • [ 6012-97-1 ]
  • [ 109384-19-2 ]
  • [ 817187-32-9 ]
YieldReaction ConditionsOperation in experiment
52% With sodium hydride In DMF (N,N-dimethyl-formamide) at 20℃; for 15h; E Method E; 1-tert-butoxycarbonyl-4-(3,4,5-trichloro-thienyloxy)-piperidine A mixture of tetrachlorothiophene (1.0 g, 4.51 mmol), 1-tert-butoxycarbonyl-4-hydroxy- piperidine (0. 91 g, 4.51 mmol), 60% sodium hydride (0.23 g, 5. 86 g) and DMF (15 ML) was stirred for 15 h at room temperature. WATER WAS ADDED (50 M)) AND THE MIXTURE was extracted with ethyl acetate (2 x 50 ml). The organic phase was washed three times with water (3 50 ml). The product was isolated as an oil. Yield 0.91 g (52%).
  • 73
  • [ 6012-97-1 ]
  • 3,4,5-trichloro-2-thiophenecarboxaldehyde [ No CAS ]
YieldReaction ConditionsOperation in experiment
84% With n-butyllithium In tetrahydrofuran; hexane; ethyl acetate; N,N-dimethyl-formamide 1 Preparation of 3,4,5-Trichloro-2-Thiophenecarboxaldehyde STR80 EXAMPLE 1 Preparation of 3,4,5-Trichloro-2-Thiophenecarboxaldehyde STR80 Butyllithium (2.5 molar in tetrahydrofuran, 3.96 mL, 9.9 mmol) is added to a solution of tetrachlorothiophene (2.00 g, 9.01 mmol) in tetrahydrofuran at 0° C. The reaction mixture is stirred at 0° C. for 30 minutes, warmed to room temperature over 45 minutes, treated with N,N-dimethylformamide (0.79 g, 10.8 mmol), stirred for three hours, poured into one molar hydrochloric acid at 4° C. and extracted with ether. The combined organic extracts are washed sequentially with water and brine, dried over MgSO4 and concentrated in vacuo to obtain a brown solid. Flash chromatography of the solid using silica gel and a 5% ethyl acetate in hexane solution gives a beige solid which is recrystallized from ethyl acetate and hexane to obtain the title product as beige needles (1.63 g, 84%, mp 81°-82° C.).
84% With n-butyllithium In tetrahydrofuran; hexane; ethyl acetate; N,N-dimethyl-formamide 1 Preparation of 3,4,5-Trichloro-2-thiophenecarboxaldehyde STR80 EXAMPLE 1 Preparation of 3,4,5-Trichloro-2-thiophenecarboxaldehyde STR80 Butyllithium (2.5 molar in tetrahydrofuran, 3.96 mL, 9.9 mmol) is added to a solution of tetrachlorothiophene (2.00 g, 9.01 mmol) in tetrahydrofuran at 0° C. The reaction mixture is stirred at 0° C. for 30 minutes, warmed to room temperature over 45 minutes, treated with N,N-dimethylformamide (0.79 g, 10.8 mmol), stirred for three hours, poured into one molar hydrochloric acid at 4° C. and extracted with ether. The combined organic extracts are washed sequentially with water and brine, dried over MgSO4 and concentrated in vacuo to obtain a brown solid. Flash chromatography of the solid using silica gel and a 5% ethyl acetate in hexane solution gives a beige solid which is recrystallized from ethyl acetate and hexane to obtain the title product as beige needles (1.63 g, 84%, mp 81°-82° C.).
  • 74
  • [ 6012-97-1 ]
  • [ 6579-01-7 ]
YieldReaction ConditionsOperation in experiment
35% With water; nitric acid for 0.0833333h; Preparation of 3 , 4-dichloro-thiophene-2, 5-dione [S compound] according to the literature: 0. Scherer, F. Kluge Chem. Ber. 99, 1966, 1973-1983; 5 g tetrachlorothiophene are stirred with 13 ml HNO3 for five minutes and the resulting brown solution is then, poured on to ice. The precipitate which has precipitated out is filtered off rapidly over a frit and recrystallized from cyclohexane. Slightly yellowish crystals are obtained in a yield of approx. 35 %.
  • 75
  • [ 6012-97-1 ]
  • KCoF4 [ No CAS ]
  • [ 699-46-7 ]
  • [ 1035801-35-4 ]
  • [ 1035953-54-8 ]
  • [ 30835-81-5 ]
YieldReaction ConditionsOperation in experiment
150-170°C;
150-170°C;
  • 76
  • [ 6012-97-1 ]
  • [ 10026-18-3 ]
  • [ 30835-81-5 ]
YieldReaction ConditionsOperation in experiment
main product: chlorofluorobutane;
main product: chlorofluorobutane;
  • 77
  • [ 6012-97-1 ]
  • mercury(II) fluoride [ No CAS ]
  • [ 699-46-7 ]
YieldReaction ConditionsOperation in experiment
0%
0%
  • 78
  • [ 6012-97-1 ]
  • silver fluoride [ No CAS ]
  • [ 699-46-7 ]
YieldReaction ConditionsOperation in experiment
0%
0%
  • 79
  • [ 6012-97-1 ]
  • [ 879-05-0 ]
  • [ 22096-15-7 ]
YieldReaction ConditionsOperation in experiment
In diethyl ether; cyclohexane addition of tetrachloro thiophene in cyclohexane to a solution of C6F5MgBr in ether, evaporation of ether and heating under reflux, 15 hours;;
In diethyl ether; cyclohexane addition of tetrachloro thiophene in cyclohexane to a solution of C6F5MgBr in ether, evaporation of ether and heating under reflux, 15 hours;;
  • 81
  • [ 6012-97-1 ]
  • [ 383-63-1 ]
  • [ 1414377-87-9 ]
YieldReaction ConditionsOperation in experiment
81.9% Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In tetrahydrofuran; hexane at -78℃; for 2h; Stage #2: ethyl trifluoroacetate, In tetrahydrofuran; hexane at -78℃; for 2.5h; 1 Preparation 1Methyl 2,2,2-trifluoro-l-(3,4,5-trichlorothiophen-2-yl)ethanoneAdd a solution of n-BuLi (21.6 mL, 2.5 M in hexane, 54.0 mmol) to a solution of2,3,4,5-tetrachloro-thiophene (10 g, 45.0 mmol) in dry THF (160 mL) at -78 °C and stir the mixture for 2 hours. Add a solution of trifluoro-acetic acid ethyl ester (9.59 g, 67.6 mmol) in THF (15 mL) and stir at -78 °C for additional 2.5 hours. Quench the reaction with saturated NH4CI solution (100 mL). Extract the aqueous mixture with EtOAc (100 mL X 3). The combined organic layers are washed with brine, dried over anhydrous Na2SC>4, and evaporate under vacuum. Purify the residue by a flash column on silica gel eluting with PE:EtOAc (10: 1 to 5: 1) to afford 2,2,2-trifluoro-l-(3,4,5-trichloro- thiophen-2-yl)-ethanone as a brown oil (10.4 g, 81.9%). 13F NMR (400 MHz, CDC13) δ -73.38 (s, 3F).
81.9% Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In tetrahydrofuran; hexane at -78℃; for 2h; Stage #2: ethyl trifluoroacetate, In tetrahydrofuran at -78℃; for 2.5h; Preparation 1Methyl 2,2,2-trifluoro-l-(3,4,5-trichlorothiophen-2-yl)ethanoneAdd a solution of n-BuLi (21.6 mL, 2.5 M in hexane, 54.0 mmol) to a solution of 2,3,4,5-tetrachloro-thiophene (10 g, 45.0 mmol) in dry THF (160 mL) at -78 °C and stir the mixture for 2 hours. Add a solution of trifluoro-acetic acid ethyl ester (9.59 g, 67.6 mmol) in THF (15 mL) and stir at -78 °C for additional 2.5 hours. Quench the reaction with saturated NH4C1 solution (100 mL). Extract the aqueous mixture with EtOAc (100 mL X 3). The combined organic layers are washed with brine, dried over anhydrous Na2S04, and evaporate under vacuum. Purify the residue by a flash column on silica gel eluting with PE:EtOAc (10: 1 to 5: 1) to afford 2,2,2-trifluoro-l-(3,4,5-trichloro- thiophen-2-yl)-ethanone as a brown oil (10.4 g, 81.9%). 13F NMR (400 MHz, CDC13) δ -73.38 (s, 3F).
81.9% Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In tetrahydrofuran; hexane at -78℃; for 2h; Stage #2: ethyl trifluoroacetate, In tetrahydrofuran; hexane at -78℃; for 2.5h; 1 Preparation 1Methyl 2,2,2-trifluoro-l-(3,4,5-trichlorothiophen-2-yl)ethanoneAdd a solution of n-BuLi (21.6 mL, 2.5 M in hexane, 54.0 mmol) to a solution of 2,3,4,5-tetrachloro-thiophene (10 g, 45.0 mmol) in dry THF (160 mL) at -78 °C and stir the mixture for 2 hours. Add a solution of trifluoro-acetic acid ethyl ester (9.59 g, 67.6 mmol) in THF (15 mL) and stir at -78 °C for additional 2.5 hours. Quench the reaction with saturated NH4C1 solution (100 mL). Extract the aqueous mixture with EtOAc (100 mL X 3). The combined organic layers are washed with brine, dried over anhydrous Na2S04, and evaporate under vacuum. Purify the residue by a flash column on silica gel eluting with PE:EtOAc (10: 1 to 5: 1) to afford 2,2,2-trifluoro-l-(3,4,5-trichloro- thiophen-2-yl)-ethanone as a brown oil (10.4 g, 81.9%). 13F NMR (400 MHz, CDC13) δ -73.38 (s, 3F).
  • 82
  • [ 6012-97-1 ]
  • [ 33513-42-7 ]
  • 3,4,5-trichloro-2-thiophenecarboxaldehyde [ No CAS ]
YieldReaction ConditionsOperation in experiment
4 g Stage #1: 2,3,4,5-tetrachlorothiophene With n-butyllithium In diethyl ether at -78 - 78℃; for 0.666667h; Inert atmosphere; Stage #2: N,N-dimethyl-formamide In diethyl ether at 20℃; for 2h; 7.1 In 250mL three bottles, under a nitrogen atmosphere, compound 7-1 (4.2 g, 19 mmol) was dissolved in diethyl ether (140 mL), cooled to below 78 ° C, n-butyllithium (2.5 M, 8.3 mL, 20.9 mmol) At -78 ° C for 40 minutes, and then a solution of N, N-dimethylformamide (2.8 g, 38 mmo 1) in ether (10 mL) was added dropwise and the reaction was allowed to proceed at room temperature for 2 hours. (50 mL) and saturated brine (50 mL). The organic phase was washed successively with water (50 mL) and saturated brine (50 mL), dried and concentrated to give 4 g of a pale yellow oil.
  • 83
  • [ 6012-97-1 ]
  • [ 106-95-6 ]
  • 2,5-diallyl-3,4-dichlorothiophene [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% Stage #1: 2,3,4,5-tetrachlorothiophene With N,N,N,N,-tetramethylethylenediamine; C4H9Mg(1+)*2C8H17O(1-)*Li(1+) In toluene at 25℃; for 4h; Schlenk technique; Inert atmosphere; Stage #2: With copper(l) iodide In toluene at 0℃; for 1h; Schlenk technique; Inert atmosphere; Stage #3: allyl bromide In toluene at 0℃; for 1h; Inert atmosphere; Schlenk technique;
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