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

HRID 1418254노트

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HRID 1418254 반응식
[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

참가 물질

4

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3e5bc6f8226f4f029ccccdc1c3ff4b44
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05882819

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