Magnesium peroxide (Mg(O2)) → HCID 118431980, compound

HRID 2207909Notes

Reaction equation

HRID 2207909 reaction equation
[Br:1][C:2]1[S:6][C:5]([CH:7]2[N:11]([C:12]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=3[F:19])[N:10]=[C:9]([CH2:20][OH:21])[CH2:8]2)=[CH:4][CH:3]=1.[O-][O-].[Mg+2]>ClCCl>[Br:1][C:2]1[S:6][C:5]([CH:7]2[N:11]([C:12]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=3[F:19])[N:10]=[C:9]([CH:20]=[O:21])[CH2:8]2)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 61745Magnesium peroxide (Mg(O2))HCID 118431940HCID 118431940, compound

Product 1

HCID 118431980HCID 118431980, compoundYield 71.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

[5-(5-Bromo-thiophen-2-yl)-1-(2,4-difluoro-phenyl)-4,5-dihydro-1H-pyrazol-3-yl]-methanol (12.9 g, 34.5 mmol) prepared in Step 4 and magnesium dioxide (MnO2) (30.0 g, 344.6 mmol) were added to dichloromethane (115.0 mL). The reaction mixture was stirred at room temperature for 3 days and then filtered to obtain a yellow filtrate. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane) to give 9.1 g of the titled compound as a yellow liquid.

Workup

  1. filtrationfiltered
  2. customto obtain a yellow filtrate
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane)

Sources & evidence

ORD record
ord-a6b4d9eb1f4e4cedace107636b0caf47
Source dataset
uspto-grants-2016_06
Patent number
US09376420B2

Reaction notes

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