Lawesson's reagent → HCID 60148827, compound

HRID 1805262Notes

Reaction equation

HRID 1805262 reaction equation
[C:1]([NH:4][NH:5][C:6]([C:8]1[C:9]([C:28]2[C:33]([F:34])=[CH:32][CH:31]=[CH:30][C:29]=2[Cl:35])=[N:10][O:11][C:12]=1[C:13]1[CH:14]=[N:15][N:16]([C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)[C:17]=1[C:18]([F:21])([F:20])[F:19])=O)(=O)[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:45])=CC=1>O1CCOCC1.ClCCl>[Cl:35][C:29]1[CH:30]=[CH:31][CH:32]=[C:33]([F:34])[C:28]=1[C:9]1[C:8]([C:6]2[S:45][C:1]([CH3:2])=[N:4][N:5]=2)=[C:12]([C:13]2[CH:14]=[N:15][N:16]([C:22]3[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=3)[C:17]=2[C:18]([F:21])([F:20])[F:19])[O:11][N:10]=1

Participants

5

Reactant 2

HCID 87949Lawesson's reagentHCID 68153191HCID 68153191, compound

Product 1

HCID 60148827HCID 60148827, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 312751,4-DioxaneSolvent

Procedure

To a solution of N′-acetyl-3-(2-chloro-6-fluorophenyl)-5-(1-(pyridin-4-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)isoxazole-4-carbohydrazide (0.029 mg, 0.01 mmol) in dioxane (1.5 mL) was added Lawesson's Reagent (23.1 mg, 0.01 mmol). The mixture was stirred at reflux for 30 min. The mixture was then diluted with dichloromethane and washed with water (3×), dried over sodium sulfate, filtered and concentrated under reduced pressure.

Workup

  1. temperatureat reflux for 30 min
  2. washwashed with water (3×)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-b8e2c318900f46479ffd976394a0de74
Source dataset
uspto-grants-2013_01
Patent number
US08354436B2

Reaction notes

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