1,1-Dichloroethane → HCID 15147116, compound

HRID 2174417Notes

Reaction equation

HRID 2174417 reaction equation
ClC(Cl)(Cl)[S:3][C:4]1[CH:22]=[CH:21][C:7]([C:8]([C:10]2[CH:15]=[CH:14][C:13]([S:16]C(Cl)(Cl)Cl)=[CH:12][CH:11]=2)=[O:9])=[CH:6][CH:5]=1.ClC(Cl)C>C(O)C>[SH:3][C:4]1[CH:22]=[CH:21][C:7]([C:8]([C:10]2[CH:15]=[CH:14][C:13]([SH:16])=[CH:12][CH:11]=2)=[O:9])=[CH:6][CH:5]=1

Participants

4

Reactant 2

HCID 63651,1-DichloroethaneHCID 86686941HCID 86686941, compound

Product 1

HCID 15147116HCID 15147116, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

10 g said 4,4′-di(trichloro methyl sulfenyl)benzophenone obtained in step 2, 30 g dichloroethane and 10 g ethanol are added into a 100 ml reaction flask. The solution is heated to react under reflux with nitrogen protection, and is cooled after reacting for 6 hours to precipitate solids. Filtering, and washing with ethanol to obtain 4.4 g white flake crystals, the yield is 85%, and the melting point is 179-182.3° C. 1H-NMR data (solvent CDCl3): δ3.6369 ppm, s, 2H, δ7.3168, 7.3435 ppm, d, 4H, δ7.6384, 7.6650 ppm, d, 4H.

Workup

  1. additionare added into a 100 ml reaction flask
  2. temperatureThe solution is heated
  3. customto react
  4. temperatureunder reflux with nitrogen protection
  5. temperatureis cooled
  6. customto precipitate solids
  7. filtrationFiltering
  8. washwashing with ethanol
  9. customto obtain 4.4 g white flake crystals

Sources & evidence

ORD record
ord-8e4a2abe6def4861b6016c474678ffcc
Source dataset
uspto-grants-2015_06
Patent number
US09061979B2

Reaction notes

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