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[ CAS No. 97-77-8 ]

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2D
Chemical Structure| 97-77-8
Chemical Structure| 97-77-8
Structure of 97-77-8 *Storage: {[proInfo.prStorage]}

Quality Control of [ 97-77-8 ]

Purity: {[proInfo.showProBatch.pb_purity]}

Related Doc. of [ 97-77-8 ]

SDS

Product Details of [ 97-77-8 ]

CAS No. :97-77-8MDL No. :MFCD00009048
Formula :C10H20N2S4Boiling Point :-
Linear Structure Formula :-InChI Key :AUZONCFQVSMFAP-UHFFFAOYSA-N
M.W :296.54Pubchem ID :3117
Synonyms :

Computed Properties of [ 97-77-8 ]

TPSA : - H-Bond Acceptor Count : -
XLogP3 : - H-Bond Donor Count : -
SP3 : - Rotatable Bond Count : -

Safety of [ 97-77-8 ]

Signal Word:DangerClass9
Precautionary Statements:P273-P280UN#:3077
Hazard Statements:H302-H317-H373-H410Packing Group:
GHS Pictogram:

Application In Synthesis of [ 97-77-8 ]

  • Downstream synthetic route of [ 97-77-8 ]

[ 97-77-8 ] Synthesis Path-Downstream   1~10

  • 2
  • [ 75-15-0 ]
  • [ 109-89-7 ]
  • [ 97-77-8 ]
YieldReaction ConditionsOperation in experiment
90% With sodium hydroxide; at 35℃; for 8h; Under a certain temperature and a certain amount of caustic and diethylamine quantitative input four flasks, and opening of the stirring, evenly mixed. Slowly dropping carbon disulfide into the four-mouth bottle in the reaction, after dropping, continuing to stir for a period of time, namely 1st step the completion of the reaction, the reaction product of the 1st step to obtain diethyl amino sodium formate. Diethylamine, sodium hydroxide and carbon disulfide molar ratio control in 1: 1.1: 1.2; the reaction temperature is 35 C; carbon disulfide increases control in between 2 h; after dropping the staying time of the control in the 6 h.2. Hold open the mixing state, under a certain temperature and a certain amount of the dispersing agent and the mild oxidizing agent dimethyl sulfoxide into four flasks, slowly dropping a certain amount of catalyst into the four-mouth bottle reaction, at the same time deep cold-acquisition and the generated gas, cryogenic storage, this component is the high value-added value by-product dimethyl sulfide. After dropping, continuing to stir for a period of time, the 2nd step the completion of the reaction, the reaction product to obtain 2nd step [...] tetraethyl thiuram disulfide. Diethyl amino sulfonic acid sodium, dimethyl sulfoxide and catalyst (to [...]) molar ratio control in 2: 1.8: 3.0; the reaction temperature control 70 C; aid the dropping time control in 2 h; after dropping the staying time of the control in the 2 h. Catalyst refers inorganically strong acid, including hydrochloric acid, dilute sulfuric acid, dilute nitric acid and the like, this embodiment uses the dilute sulfuric acid. Dispersing agent means a surface active agent, including dodecyl benzene benzene sulfonic acid sodium, such as EDTA, the embodiment using sodium dodecyl benzene sulfonate. The amount of the dispersing agent for the solution quality 1/10000 - 1/100, in this embodiment 1/1000.3. After the reaction is finished, the mixture is filtered, the filter cake washing with clear water 3 times, 60 - 80 C drying, drying time is 4 - 12 is H, to obtain the target product [...] tetraethyl thiuram class. The reaction yield can be 90%, HPLC purity of the product test to 94%.
86% Analogs of [97-77-8]disulfiram are prepared in a manner similar to the synthesis of [97-77-8]disulfiram, whose synthesis is as follows: A solution of diethylamine (10.0 g, 0.137 mol) in 100 ML of water is treated with 13.7 ML of 1.0M NaOH. carbon disulfide (8.24 ML, 0.137 mol) is added dropwise and the solution was stirred for 1 hr.The solution is cooled with an ice bath and 15.5 ML of 30% hydrogen peroxide is added dropwise while keeping the temperature of the reaction mixture below 10 C. The reaction mixture is stirred for 4 hours at 0 C. and the resulting off-white solid is filtered and collected to yield [97-77-8]disulfiram (35.0 g, 86% yield).
55% With dihydrogen peroxide; In methanol; water;Inert atmosphere; Cooling; Heating; To a solution of diethylamine (7 mL, 67 mmol) in methanol(50 mL) upon cooling with room temperature water bath was added dropwise CS2 (4.3 mL, 71 mmol), and then hydrogen peroxide (3.1 mL of 12 M aqueous solution, 37 mmol) which caused the formation of the precipitate. The mixture was heated until dissolution of the precipitate. The mixture was allowed cool slowly to 5 C. The crystals was filtered, washed with methanol, and dried under vacuum. Yield 5.5 g (55%). Mp 69-71 C [19].
  • 3
  • [ 97-77-8 ]
  • [ 621-82-9 ]
  • [ 27829-46-5 ]
YieldReaction ConditionsOperation in experiment
66% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; Add 0.5mmol of cinnamic acid and 0.55mmol of tetraethylthiuram disulfide0.5 ~ 1ml of dichloroethane to make a mixture, the mixture was placed in 5mlInside the Schlenk tube, put it in an oil bath at 90 100 ,After 36 to 48 hours of reaction, cool to room temperature to obtain a reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,Thin layer chromatography was performed to obtain 67.0 mg of the target product.
  • 4
  • [ 95-20-5 ]
  • [ 97-77-8 ]
  • 2-methyl-1H-indol-3-yl N,N-diethylaminodithioformate [ No CAS ]
  • 5
  • [ 148-18-5 ]
  • [ 97-77-8 ]
Reference: [1]Synthesis,2002,p. 2513 - 2516
[2]Journal of the American Chemical Society,2017,vol. 139,p. 15530 - 15538
[3]Journal of Porphyrins and Phthalocyanines,2015,vol. 19,p. 1159 - 1167
[4]Journal of Porphyrins and Phthalocyanines,2017,vol. 21,p. 37 - 47
[5]Synthetic Communications,2001,vol. 31,p. 1477 - 1480
[6]Journal of Organic Chemistry,1988,vol. 53,p. 2119 - 2120
[7]RSC Advances,2014,vol. 4,p. 40054 - 40060
[8]Recueil des Travaux Chimiques des Pays-Bas,1954,vol. 73,p. 561
[9]Journal of the Chemical Society,1959,p. 2749,2752
[10]Journal of general chemistry of the USSR,1991,vol. 61,p. 739 - 742
    Zhurnal Obshchei Khimii,1991,vol. 61,p. 818 - 821
[11]Journal of the American Chemical Society,1986,vol. 108,p. 3570 - 3577
[12]Russian Chemical Bulletin,1999,vol. 48,p. 2073 - 2076
[13]Petroleum Chemistry,2013,vol. 53,p. 197 - 200
    Neftekhimiya,2013,vol. 53,p. 221 - 225,5
[14]Russian Journal of Physical Chemistry,2014,vol. 88,p. 2064 - 2067
    Zh. Fiz. Khim.,2014,vol. 88,p. 41904 - 41907
[15]Journal of Porphyrins and Phthalocyanines,2015,vol. 19,p. 573 - 581
[16]Journal of Porphyrins and Phthalocyanines,2015,vol. 19,p. 983 - 996
[17]Journal of Inclusion Phenomena and Macrocyclic Chemistry,2017,vol. 87,p. 37 - 43
[18]Russian Chemical Bulletin,2016,vol. 65,p. 2220 - 2228
    Izv. Akad. Nauk, Ser. Khim.,2016,p. 2220 - 2228,9
[19]Journal of Molecular Structure,2017,vol. 1149,p. 17 - 26
[20]Russian Journal of General Chemistry,2018,vol. 88,p. 742 - 750
    Zh. Obshch. Khim.,2018,vol. 88,p. 742 - 750,9
[21]Russian Journal of General Chemistry,2018,vol. 88,p. 751 - 757
    Zh. Org. Khim.,2018,vol. 88,p. 672 - 678,7
  • 6
  • [ 97-77-8 ]
  • [ 65-85-0 ]
  • [ 1696-17-9 ]
YieldReaction ConditionsOperation in experiment
58% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; 0.5mmol of benzoic acid and 0.55mmol of tetraethylthiuram disulfide are added to 0.5 to 1ml of dichloroethane to make a mixture, and the mixture is placed in 5ml of SchlenkInside the tube, put it in an oil bath at 90 100 and heat it for 36 48h.Cool to room temperature to obtain the reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,TLC separation was performed to obtain 51.3 mg of the target product.
  • 7
  • [ 97-77-8 ]
  • [ 1124-65-8 ]
  • [ 88312-34-9 ]
YieldReaction ConditionsOperation in experiment
66% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; Take 3- (2-thienyl) acrylic acid 0.5mmol, tetraethylthiuram disulfide0.55mmol was added into 0.5 1ml of dichloroethane to make a mixture,Place the mixture in a 5ml Schlenk tube,Put it in an oil bath at 90 100 , after 36 48h reaction,Cool to room temperature to obtain the reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,TLC separation was performed to obtain 69.0 mg of the target product.
  • 8
  • [ 97-77-8 ]
  • [ 539-47-9 ]
  • [ 88312-33-8 ]
YieldReaction ConditionsOperation in experiment
50% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; Add 0.5 mmol of 3- (2-furyl) acrylic acid and 0.55 mmol of tetraethylthiuram disulfide to 0.5 to 1 ml of dichloroethane to make a mixture,Place the mixture in a 5ml Schlenk tube,Put it in an oil bath at 90 100 , after 36 48h reaction,Cool to room temperature to obtain the reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,TLC separation gave 48.3 mg of target product.
  • 9
  • [ 97-77-8 ]
  • [ 1866-38-2 ]
  • [ 1085449-78-0 ]
YieldReaction ConditionsOperation in experiment
49% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; Add 0.5mmol of 3-chlorocinnamic acid and 0.55mmol of tetraethylthiuram disulfideMake a mixture in 0.5 to 1 ml of dichloroethane, put the mixture in a 5 ml Schlenk tube, and heat it in an oil bath at 90 to 100 C.After 36 to 48 hours of reaction, cool to room temperature to obtain a reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,TLC separation gave 60.0 mg of the target product.
  • 10
  • [ 97-77-8 ]
  • [ 2062-26-2 ]
  • [ 1184304-16-2 ]
YieldReaction ConditionsOperation in experiment
55% In 1,2-dichloro-ethane; at 90 - 100℃;Schlenk technique; Add 0.5 mmol of 4-trifluoromethylcinnamic acid and 0.55 mmol of tetraethylthiuram disulfide to 0.5 to 1 ml of dichloroethane to make a mixture,Place the mixture in a 5ml Schlenk tube,Put it in an oil bath at 90 100 , after 36 48h reaction,Cool to room temperature to obtain the reaction solution;(2) The reaction solution obtained in step (1) is directly concentrated to obtain a concentrate,The concentrate was made with ethyl acetate / petroleum ether = 2/1 (v / v) as the developing agent,Perform TLC separation,74.6 mg of target product was obtained.
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