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

HRID 436220
ノート
印刷プレビュー

反応式

HRID 436220 の反応式
[C:1](Cl)(Cl)=[O:2].[CH3:5][S:6]([C:9]1[S:13][C:12]([NH2:14])=[N:11][N:10]=1)(=[O:8])=[O:7]>C(OCC)(=O)C>[CH3:5][S:6]([C:9]1[S:13][C:12]([N:14]=[C:1]=[O:2])=[N:11][N:10]=1)(=[O:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6371PhosgeneHCID 164543745-(Methanesulfonyl)-1,3,4-thiadiazol-2-amine

生成物 1

HCID 542537365-Methylsulfonyl-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 glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-methylsulfonyl-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-methylsulfonyl-1,3,4-thiadiazol-2-yl isocyanate dimer.

このページの内容参加物実験手順後処理出典と根拠反応ノート

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-7b06133b42434fe0a590ecb4f60a22cd
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04008068

反応ノート

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