HCID 13781851, compound → HCID 14121497, compound

HRID 648431Notes

Reaction equation

HRID 648431 reaction equation
[CH2:1]([S:8]([C:11]1[C:25]([OH:26])=[C:24]([C:27]([O:29][CH:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)=[O:28])[CH:23]=[C:22]([OH:36])[C:12]=1[C:13]([O:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1)=[O:14])(=[O:10])=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>[O-2].[O-2].[Mn+4].C1(C)C=CC=CC=1>[CH2:1]([S:8]([C:11]1[C:25](=[O:26])[C:24]([C:27]([O:29][CH:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)=[O:28])=[CH:23][C:22](=[O:36])[C:12]=1[C:13]([O:15][CH:16]1[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]1)=[O:14])(=[O:10])=[O:9])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 1

HCID 13781851HCID 13781851, compound

Product 1

HCID 14121497HCID 14121497, compoundYield 60%

Reagents, catalysts & solvents 2

HCID 178418406HCID 178418406, compoundCatalystHCID 1140TolueneSolvent

Procedure

One part of dicyclohexyl 2-benzylsulfonyl-3,6-dihydroxyterephthalate, 2 parts of electrolytic manganese dioxide and 3 parts of toluene were agitated at 35°-45° C. for 8 hours and then at its boiling point for additional 2 hours. The reaction mixture was hotfiltered and the volume of the resultant filtrate was concentrated to about 1/3. After adding ligroin to the concentrate, the resultant mixture was allowed to cool to obtain light-yellowish crystals with a yield of 60%. Upon recrystallization, they showed a melting point of 160°-162° C. Detailed analysis data of this compound, such as its elementary analysis data, are as described before.

Workup

  1. concentrationthe volume of the resultant filtrate was concentrated to about 1/3
  2. additionAfter adding ligroin to the concentrate
  3. temperatureto cool
  4. customto obtain light-yellowish crystals with a yield of 60%
  5. customUpon recrystallization, they

Sources & evidence

ORD record
ord-28b1ffa174a74b00ab8b6052cd6275a8
Source dataset
uspto-grants-1988_04
Patent number
US04735744

Reaction notes

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