Sulfuryl chloride → HCID 22912800, compound

HRID 1653950Notes

Reaction equation

HRID 1653950 reaction equation
[NH2:1][C:2]1[N:6]([C:7]2[CH:11]=[C:10]([O:12][CH:13]([F:15])[F:14])[N:9]([CH3:16])[N:8]=2)[N:5]=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18].S(Cl)([Cl:23])(=O)=O>C(Cl)Cl>[NH2:1][C:2]1[N:6]([C:7]2[C:11]([Cl:23])=[C:10]([O:12][CH:13]([F:14])[F:15])[N:9]([CH3:16])[N:8]=2)[N:5]=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18]

Participants

4

Reactant 2

HCID 24648Sulfuryl chlorideHCID 15767491HCID 15767491, compound

Product 1

HCID 22912800HCID 22912800, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.5 g (5.5 mmole) 5-Amino-4-nitro-1-(1-methyl-5-difluoromethoxy-3-pyrazolyl)pyrazole in 30 ml methylene chloride was treated with 0.74 g (5.5 mmole) sulfuryl chloride and the mixture stirred for 10 minute sat room temperature. It was then concentrated and the residue was recrystallised from diisopropyl ether/ethyl acetate. The mother liquor was concentrated and chromatographed (SiO2 /hexane/ethyl acetate 3:1).

Workup

  1. customsat room temperature
  2. concentrationIt was then concentrated
  3. customthe residue was recrystallised from diisopropyl ether/ethyl acetate
  4. concentrationThe mother liquor was concentrated
  5. customchromatographed (SiO2 /hexane/ethyl acetate 3:1)

Sources & evidence

ORD record
ord-a9c163ae96714f23ae293edec9c54d80
Source dataset
uspto-grants-1995_04
Patent number
US05405829

Reaction notes

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