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Chemical Structure| 69815-97-0 Chemical Structure| 69815-97-0

Structure of 69815-97-0

Chemical Structure| 69815-97-0

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Product Details of [ 69815-97-0 ]

CAS No. :69815-97-0
Formula : C5H5ClO2S2
M.W : 196.68
SMILES Code : O=S(C1=CC(C)=CS1)(Cl)=O
MDL No. :MFCD05864497

Safety of [ 69815-97-0 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H314
Precautionary Statements:P260-P280-P303+P361+P353-P301+P330+P331-P304+P340+P310-P305+P351+P338+P310
Class:8
UN#:3261
Packing Group:

Application In Synthesis of [ 69815-97-0 ]

* 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 [ 69815-97-0 ]

[ 69815-97-0 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 69815-97-0 ]
  • [ 1597-32-6 ]
  • N-(6-fluoropyridin-2-yl)-4-methyl-5-nitrothiophene-2-sulfonamide [ No CAS ]
YieldReaction ConditionsOperation in experiment
45% To a solution of 4-methylthiophene-2-sulfonyl chloride (13.9 g, 66.1 mmol) in anhydrous dichloromethane (5.5 ml_) was carefully added concentrated nitric acid (5.5 ml_) and concentrated sulfuric acid (0.5 ml_) at 0 C. The reaction mixture was allowed to warm to ambient temperature and stirred for 2 hours. The reaction mixture was diluted with ethyl acetate (25 ml_), and carefully neutralized with saturated sodium bicarbonate solution (100 ml_). The aqueous layer was extracted with ethyl acetate (3 x 50 ml_), and the combined organic layers were washed with saturated sodium bicarbonate solution (50 ml_), water (50 ml_), and brine (50 ml_). The combined organic layers were dried over anhydrous magnesium sulfate, filtered, and the filtrate concentrated in vacuo. The residue was dissolved in anhydrous dichloromethane (20 ml_) and slowly added to a solution of <strong>[1597-32-6]6-fluoropyridin-2-amine</strong> (1.5 g, 13.5 mmol) in pyridine (20 ml_) at 0 C. The reaction mixture was stirred at 0 C for 3 hours. The reaction mixture was then diluted with ethyl acetate (200 ml_) and washed with 1 M hydrochloric acid (3 c 50 ml_), water (50 ml_), and brine (50 ml_). The organic phase was dried over anhydrous magnesium sulfate, filtered, and the filtrate concentrated in vacuo. Purification of the residue by column chromatography, eluting with ethyl acetate (containing 10% of 2-propanol and 10% of triethylamine) in heptane, afforded the title compound as an orange oil (1.75 g, 45% yield): 1H NMR (300 MHz, CDCI3) d 7.51 (dt, J = 9.1 , 7.9 Hz, 1 H), 7.31 (d, J = 0.4 Hz, 1 H), 6.96 (ddd, J = 8.0, 2.7, 0.5 Hz, 1 H), 6.28 (ddd, J = 7.8, 2.7, 0.5 Hz, 1 H), 2.58 (d, J = 0.4 Hz, 3H), NH not observed.
 

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