Phosgene → 5-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

HRID 596738ノート

反応式

HRID 596738 の反応式
[C:1](Cl)(Cl)=[O:2].[CH:5]1([C:12]2[S:16][C:15]([NH2:17])=[N:14][N:13]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1>C(OCC)(=O)C>[CH:5]1([C:12]2[S:16][C:15]([N:17]=[C:1]=[O:2])=[N:14][N:13]=2)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]1

参加物

4

反応物 2

HCID 6371PhosgeneHCID 214478325-Cycloheptyl-2-amino-1,3,4-thiadiazole

生成物 1

HCID 214819185-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A saturated solution of phosgene in ethyl acetate (100 ml) is charged into a class reaction vessel equipped with a mechanical stirrer. A slurry of 5-cycloheptyl-2-amino-1,3,4-thiadiazole (50 grams) in ethyl acetate (300 ml) is added to the reaction vessel and the resulting mixture is stirred for a period of about 16 hours, resulting in the formation of a precipitate. The reaction mixture is then purged with nitrogen gas to remove unreacted phosgene. The purged mixture is then filtered to recover the precipitate. The precipitate is then recrystallized to yield the desired product 5-cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate dimer.

後処理

  1. customequipped with a mechanical stirrer
  2. customresulting in the formation of a precipitate
  3. customThe reaction mixture is then purged with nitrogen gas
  4. customto remove unreacted phosgene
  5. filtrationThe purged mixture is then filtered
  6. customto recover the precipitate
  7. customThe precipitate is then recrystallized

出典と根拠

ORDレコード
ord-9f58ca8b0e654924b6a056ed727eaf31
出典データセット
uspto-grants-1977_03
特許番号
US04012223

反応ノート

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