HCID 13764021, compound → HCID 13764031, compound

HRID 1982543Notes

Reaction equation

HRID 1982543 reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]3[N:10]([CH:14]=[CH:15][N:16]=3)[CH2:11][CH2:12][CH:13]=2)=[CH:4][CH:3]=1>C(Cl)Cl.[O-2].[O-2].[Mn+4]>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]3[N:10]([CH:14]=[CH:15][N:16]=3)[CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

Participants

4

Reactant 1

HCID 13764021HCID 13764021, compound

Product 1

HCID 13764031HCID 13764031, compound

Reagents, catalysts & solvents 2

HCID 178418406HCID 178418406, compoundCatalystHCID 6344DichloromethaneSolvent

Procedure

Combine 30 g (0.14 mole) of the product from Example 22 with 150 g of "activated" manganese dioxide in 500 ml of methylene chloride and heat to reflux for 6 hr. Filter the reaction mixture over celite, dry over magnesium sulfate, treat with charcoal, and remove the solvent in vacuo. Crystallize the residue from ether to provide the title compound.

Workup

  1. temperatureto reflux for 6 hr
  2. filtrationFilter the reaction mixture over celite,
  3. dry with materialdry over magnesium sulfate
  4. additiontreat with charcoal
  5. customremove the solvent in vacuo
  6. customCrystallize the residue from ether

Sources & evidence

ORD record
ord-692428075dfb4ea59e31d48dac6a844a
Source dataset
uspto-grants-1986_06
Patent number
US04596872

Reaction notes

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