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Acetyl chloride → Methyl-N-acetyl-1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate

HRID 2253669
ノート
印刷プレビュー

反応式

HRID 2253669 の反応式
I.[CH3:2][S:3][C:4]([N:6]([CH3:15])[N:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[NH:5].C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24]>ClCCl>[CH3:2][S:3][C:4]([N:6]([CH3:15])[N:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[N:5][C:23](=[O:25])[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 70433894Methyl-1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate-hydroiodide

生成物 1

HCID 54432660Methyl-N-acetyl-1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methyl-1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate-hydroiodide* (4 g) and triethylamine (2.5 g) were dissolved in dichloromethane (50 ml). To this solution acetyl chloride (1.05 g) was added slowly maintaining temperature below 20° C. The mixture was stirred at room temperature in a dry nitrogen atmosphere for 1.5 h. The organic residues were washed with water (5×20 ml), dried over anhydrous sodium sulphate and the solvent removed in vacuo giving a yellow solid which upon trituration with ether gave the title compound (2.30 g) as an off-white solid of m.pt. 102°-104° C.

後処理

  1. temperaturemaintaining temperature below 20° C
  2. washThe organic residues were washed with water (5×20 ml)
  3. dry with materialdried over anhydrous sodium sulphate
  4. customthe solvent removed in vacuo
  5. customgiving a yellow solid which upon trituration with ether

出典と根拠

ORDレコード
ord-405d644f544b4767ab2ea47b264b90cb
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05232938

反応ノート

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