Chloroform → 497851-82-8
Reaction equation
[CH2:1]([S:3][C:4]1[N:5]([CH2:11][CH:12]([CH3:14])[CH3:13])[C:6](CO)=[N:7][N:8]=1)[CH3:2].[CH:15]([Cl:18])(Cl)[Cl:16]>S(Cl)(Cl)=O>[ClH:16].[Cl:18][CH2:15][C:6]1[N:5]([CH2:11][CH:12]([CH3:14])[CH3:13])[C:4]([S:3][CH2:1][CH3:2])=[N:8][N:7]=1Participants
4
Reagents, catalysts & solvents 1
Procedure
To a solution of 5-ethylthio-3-hydroxymethyl-4-isobutyl-4H-1,2,4-triazole (1.0 g) in chloroform (3 ml), thionyl chloride (8 ml) was slowly added at 0° C. The mixture was heated to reflux for 1 hour, and concentrated under reduced pressure. To the residue was added diethylether, and the precipitated crystals were collected by filtration. The crystals were washed with diethylether, to give 3-chloromethyl-5-ethylthio-4-isobutyl-4H-1,2,4-triazole hydrochloride (0.64 g) as colorless crystals.
Workup
- temperatureThe mixture was heated
- temperatureto reflux for 1 hour
- concentrationconcentrated under reduced pressure
- additionTo the residue was added diethylether
- filtrationthe precipitated crystals were collected by filtration
- washThe crystals were washed with diethylether
Sources & evidence
- ORD record
- ord-3e005e4993c146f4bcd35f9120be285e
- Source dataset
- uspto-grants-2007_08
- Patent number
- US07262185B2
Reaction notes
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