Hydrogen Peroxide → 2-methyl-5-[(5-methyl-1,3,4-thiadiazol-2-yl)disulfanyl]-1,3,4-thiadiazole
Reaction equation
[SH:1][C:2]1[S:3][C:4]([CH3:7])=[N:5][N:6]=1.OO>CO>[CH3:7][C:4]1[S:3][C:2]([S:1][S:1][C:2]2[S:3][C:4]([CH3:7])=[N:5][N:6]=2)=[N:6][N:5]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Within a flask having a capacity of 1000 ml, 2-mercapto-5-methyl-1,3,4-thiadiazole of 150 mmol is solved in methanol of 450 ml. Into the solution thus prepared, 34.5% hydrogen peroxide of 39 ml is dropped slowly. The solution was stirred for one hour at room temperature. Thereafter, by decompression and heating, precipitate was created. The solution was filtered and washed. By the subsequent drying in a decompressing atmosphere, crude crystal was obtained. By recrystallization using ethanol, 5,5'-dithiobis (5-methyl-1,3,4-thiadiazole) (hereinafter referred to as "active material ε") was obtained.
Workup
- customWithin a flask having
- customInto the solution thus prepared
- temperatureThereafter, by decompression and heating
- filtrationThe solution was filtered
- washwashed
- customBy the subsequent drying in a decompressing atmosphere
- customcrude crystal was obtained
- customBy recrystallization
- customwas obtained
Sources & evidence
- ORD record
- ord-3e5bc6f8226f4f029ccccdc1c3ff4b44
- Source dataset
- uspto-grants-1999_03
- Patent number
- US05882819
Reaction notes
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