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[ CAS No. 39076-88-5 ] {[proInfo.proName]}

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3d Animation Molecule Structure of 39076-88-5
Chemical Structure| 39076-88-5
Chemical Structure| 39076-88-5
Structure of 39076-88-5 * Storage: {[proInfo.prStorage]}
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Product Details of [ 39076-88-5 ]

CAS No. :39076-88-5 MDL No. :
Formula : C6H2Cl2S2 Boiling Point : -
Linear Structure Formula :- InChI Key :DWPMHGKBWNDQQO-UHFFFAOYSA-N
M.W : 209.12 Pubchem ID :51350849
Synonyms :

Safety of [ 39076-88-5 ]

Signal Word:Danger Class:6.1
Precautionary Statements:P264-P270-P301+P310+P330-P405-P501 UN#:2811
Hazard Statements:H301 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 39076-88-5 ]

* 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 [ 39076-88-5 ]

[ 39076-88-5 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 251-41-2 ]
  • [ 39076-88-5 ]
YieldReaction ConditionsOperation in experiment
90.4% With N-chloro-succinimide; In N,N-dimethyl-formamide; at 25℃; Take a single-necked round-bottomed flask, add N-chlorosuccinimide to the N, N-dimethylformamide solution of thiophene and stir at room temperature for several hours. Monitor by TLC. After the reaction is completed, quench with water and quench The liquid was transferred to a separatory funnel and extracted with ether. The organic phase was dried over anhydrous sodium sulfate. After spinning, it was passed through the column with petroleum ether eluent to obtain a white solid, namely bilateral chlorothiophene product 1; of which, N-chloro The ratio of succinimide, thiophene, and N, N-dimethylformamide is 10-20 mmol: 20-50 mmol: 40-100 mL; the yield is 90.4%
  • 2
  • [ 39076-88-5 ]
  • [ 1268375-33-2 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1.1: 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride / tetrahydrofuran / 25 °C / Inert atmosphere 1.2: 1 h / -40 - 20 °C / Inert atmosphere 2.1: 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride / tetrahydrofuran / -20 °C / Inert atmosphere 2.2: 12 h / -20 - 20 °C / Inert atmosphere
Multi-step reaction with 2 steps 1.1: 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex / tetrahydrofuran / 20 °C / Inert atmosphere 1.2: -80 - 0 °C 2.1: 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex / tetrahydrofuran / -20 °C
  • 3
  • [ 39076-88-5 ]
  • [ 541-41-3 ]
  • [ 1268375-33-2 ]
YieldReaction ConditionsOperation in experiment
91% With 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex In tetrahydrofuran at 5 - 23℃; for 43h; 81 Intermediate 9 To a solution of 2,5-dichloro-thieno[3,2-b]thiophene (17.3 g, 82.7 mmol) in anhydrous tetrahydrofuran (173 cm3) at 5 °C is added ethyl chloroformate (23.7 cm3, 248 mmol). A solution of 2,2,6,6- tetramethylpiperidinylmagnesium chloride lithium chloride complex (207 cm3; 207 mmol, 1 .0 M in tetrahydrofuran) is then added dropwise over 1 hour. The reaction is slowly warmed to 23 °C and stirred for 42 hours. Water (200 cm3) is added, the mixture stirred for 10 minutes and the solid collected by filtration and washed with water (2 x 100 cm3). The solid is triturated in acetone (200 cm3), the solid collected by filtration and washed with acetone (2 x 100 cm3) to give intermediate (26.6 g, 91 %) as a white solid. 1H N MR (400 MHz, CDCIs) 4.46 (4H, q, J 7.1 ), 1 .47 (6H, t, J 7.1 ).
91% With 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex In tetrahydrofuran at 0 - 23℃; for 43h; 1 Intermediate 1 To a solution of 2,5-dichloro-thieno[3,2-b]thiophene (17.3 g, 82.7 mmol) in anhydrous tetrahydrofuran (173 cm3) at 5° C. is added ethyl chloroformate (23.7 cm3, 248 mmol). A solution of 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex (207 cm3, 207 mmol, 1.0 M in tetrahydrofuran) is then added dropwise over 1 hour. The reaction is slowly warmed to 23° C. and stirred for 42 hours. Water (200 cm3) is added, the mixture stirred for 10 minutes and the solid collected by filtration and washed with water (2×100 cm3). The solid is triturated in acetone (200 cm3), collected by filtration and washed with acetone (2×100 cm3) to give intermediate 1 (26.6 g, 91%) as a white solid. 1H NMR (400 MHz, CDCl3) 4.46 (4H, q, J 7.1), 1.47 (6H, t, J 7.1).
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