Hydrogen Peroxide → 2-methyl-5-[(5-methyl-1,3,4-thiadiazol-2-yl)disulfanyl]-1,3,4-thiadiazole

HRID 1418254ノート

反応式

HRID 1418254 の反応式
[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]=1

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 178434161HCID 178434161、化合物

生成物 1

HCID 52329992-methyl-5-[(5-methyl-1,3,4-thiadiazol-2-yl)disulfanyl]-1,3,4-thiadiazole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  1. customWithin a flask having
  2. customInto the solution thus prepared
  3. temperatureThereafter, by decompression and heating
  4. filtrationThe solution was filtered
  5. washwashed
  6. customBy the subsequent drying in a decompressing atmosphere
  7. customcrude crystal was obtained
  8. customBy recrystallization
  9. customwas obtained

出典と根拠

ORDレコード
ord-3e5bc6f8226f4f029ccccdc1c3ff4b44
出典データセット
uspto-grants-1999_03
特許番号
US05882819

反応ノート

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