Water → HCID 66839038, compound

HRID 546777Notes

Reaction equation

HRID 546777 reaction equation
[C:1]1([CH3:29])[CH:6]=[CH:5][C:4]([S:7][CH2:8][CH2:9][C:10]2[N:28]=[C:13]3[CH:14]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[C:24]([F:27])([F:26])[F:25])[CH2:15][CH2:16][CH2:17][N:12]3[N:11]=2)=[CH:3][CH:2]=1.C(OCC)(=[O:32])C.O>CO.O>[C:1]1([CH3:29])[CH:6]=[CH:5][C:4]([S:7]([CH2:8][CH2:9][C:10]2[N:28]=[C:13]3[CH:14]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[C:24]([F:26])([F:27])[F:25])[CH2:15][CH2:16][CH2:17][N:12]3[N:11]=2)=[O:32])=[CH:3][CH:2]=1

Participants

5

Reactant 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 66839211HCID 66839211, compound

Product 1

HCID 66839038HCID 66839038, compound

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Procedure

2-(2-p-Tolylsulfanylethyl)-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro[1,2,4]triazolo[1,5-a]pyridine (8.8 g) was dissolved in a mixed solvent of methanol-water (2:1 v/v) (300 ml). Sodium periodide (6.78 g) was added under cooling with an ice water bath, and the reaction solution was stirred at room temperature overnight. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration and the organic layer was concentrated under reduced pressure to obtain the title compound (8.87 g). The property values of the compound are as follows.

Workup

  1. temperatureunder cooling with an ice water bath
  2. customthe organic layer was separated
  3. washThe resulting organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe drying agent was separated by filtration
  6. concentrationthe organic layer was concentrated under reduced pressure

Sources & evidence

ORD record
ord-b911c4ebffc94cbdbc8633369b8bf1b6
Source dataset
uspto-grants-2011_05
Patent number
US07935815B2

Reaction notes

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