Dichloromethane → HCID 86755341, compound

HRID 1005287Notes

Reaction equation

HRID 1005287 reaction equation
CS[S:3][CH3:4].N(O[C:8](C)(C)C)=O.NC1C(Cl)=C[C:16]([Cl:33])=[C:17]([C:19]2[C:23]([C:24]([F:27])([F:26])[F:25])=[C:22]([C:28]([F:31])([F:30])[F:29])[N:21]([CH3:32])[N:20]=2)C=1.Cl[CH2:36][Cl:37]>>[Cl:33][C:16]1[S:3][C:4]([CH3:8])=[C:36]([Cl:37])[C:17]=1[C:19]1[C:23]([C:24]([F:26])([F:27])[F:25])=[C:22]([C:28]([F:29])([F:30])[F:31])[N:21]([CH3:32])[N:20]=1

Participants

5

Reactant 4

HCID 6344DichloromethaneHCID 10906Tert-Butyl nitriteHCID 12232Dimethyl DisulfideHCID 18791026HCID 18791026, compound

Product 1

HCID 86755341HCID 86755341, compoundYield 37%

Procedure

1.5 g (16 mmol) of dimethyl disulfide and 5.3 g (52 mmol) of tert-butyl nitrite were added to a solution of 2 g (5.3 mmol) of 3-(5-amino-2,4-dichlorophenyl)-1-methyl-4,5-di(trifluoromethyl)-1H-pyrazole in 30 ml of dichloromethane. The reaction mixture was subsequently stirred for 16 hours, whereupon it was washed with water and dilute sodium hydroxide solution, dried over magnesium sulfate and finally concentrated. The residue was purified by means of silica gel chromatography (eluent: hexane/ethyl acetate =4:1). Yield: 37%.

Workup

  1. washwas washed with water and dilute sodium hydroxide solution
  2. dry with materialdried over magnesium sulfate
  3. concentrationfinally concentrated
  4. customThe residue was purified by means of silica gel chromatography (eluent: hexane/ethyl acetate =4:1)

Sources & evidence

ORD record
ord-53a8cd16f0b44e49bdaee94fff40086f
Source dataset
uspto-grants-2000_04
Patent number
US06054412

Reaction notes

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