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Chemical Structure| 385765-64-0 Chemical Structure| 385765-64-0

Structure of 385765-64-0

Chemical Structure| 385765-64-0

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Product Details of [ 385765-64-0 ]

CAS No. :385765-64-0
Formula : C12H5Cl2F6N3O3S
M.W : 456.15
SMILES Code : O=C(C1=NN(C2=C(Cl)C=C(C(F)(F)F)C=C2Cl)C(N)=C1S(C(F)(F)F)=O)O
MDL No. :N/A

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Application In Synthesis of [ 385765-64-0 ]

* 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 [ 385765-64-0 ]

[ 385765-64-0 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 120068-37-3 ]
  • [ 385765-64-0 ]
YieldReaction ConditionsOperation in experiment
72% With sulfuric acid; acetic acid; In water; at 120℃;Reflux; <strong>[120068-37-3]Fipronil</strong> (8.74 g, 20 mmol) was dissolved in acetic acid (50 mL). Concentrated (98%) sulfuric acid(25 mL) and water (20 mL) was then added, and the mixture was stirred at 120 C for 1 h and thenheated to reflux for an additional 2 h. After cooling to room temperature, 1 M aqueous solution ofsodium hydroxide was added dropwise at 0 C until the pH reached 10. Water was added to dissolveall precipitate, and the aqueous solution was washed with ethyl ether (3 200 mL). The aqueous layerwas acidified with 1 M hydrochloric acid solution until the pH reached 1, and was then extractedwith ethyl acetate (3 200 mL). The combined organic layer was washed with brine (3 200 mL),dried over anhydrous sodium sulphate, and evaporated under reduced pressure. The residue wasrecrystallized with mixture of ethyl acetate (5 mL) and petroleum ether (150 mL) twice and dried under vacuum to afford compound 2. The 1H-NMR and 13C-NMR spectra of compound 2 can be found inFigures S1 and S2. Off-white solid, yield 72%, m.p. 154-156 C. 1H-NMR (600 MHz, DMSO-d6) delta 13.75(s, 1H), 8.27 (s, 2H), 6.81 (s, 2H). 13C-NMR (150 MHz, DMSO-d6) delta 161.74, 152.10, 143.75, 136.21, 135.93,135.25, 133.05 (q, J = 33.8 Hz), 126.68-126.42, 126.16 (q, J = 340.7 Hz), 122.36 (q, J = 273.9 Hz), 88.63.ESI-HRMS calcd for C12H6Cl2F6N3O3S [M + H]+ 455.9411; found, 455.9424.
 

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