HCID 86686940, compound → HCID 86686939, compound

HRID 2174415Notes

Reaction equation

HRID 2174415 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:21])[C:10]2[CH:15]=[CH:14][C:13]([S:16]C(Cl)(Cl)Cl)=[CH:12][CH:11]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=1>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:21])[C:10]2[CH:11]=[CH:12][C:13]([SH:16])=[CH:14][CH:15]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=1

Participants

3

Reactant 1

HCID 86686940HCID 86686940, compound

Product 1

HCID 86686939HCID 86686939, compoundYield 73.5%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In a 100 ml three-neck flask, said 3′,5′-dichloro-4-(trichloro methyl sulfenyl)benzophenone is added into 80 g methanol. The solution is heated with stirring under nitrogen protection to reflux for 5 h, and then is distilled to remove the methanol and all low-boiling-point substances. The residue is recrystallized in a mixed solvent consisting of ethyl acetate and petroleum ether in a weight ratio 1:1 to obtain 21 g yellow-green needle-like crystals with a purity of 98.8%, the yield is 73.5%, and the melting point is 98-99° C. 1H-NMR data (solvent CDCl3): δ3.6808 ppm, s, 1H, δ7.3431, 7.3700 ppm, d, 2H, δ7.5665, 7.5702 ppm, d, 1H, δ7.6033, 7.6065 ppm, d, 2H, 7.6489, 7.6758 ppm, d, 2H.

Workup

  1. customIn a 100 ml three-neck flask, said
  2. temperatureThe solution is heated
  3. temperatureto reflux for 5 h
  4. distillationis distilled
  5. customto remove the methanol
  6. customThe residue is recrystallized in a mixed solvent

Sources & evidence

ORD record
ord-34c3c9546e454bbe8e4d4b9f33fd9ff3
Source dataset
uspto-grants-2015_06
Patent number
US09061979B2

Reaction notes

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