Methyl iodide → 3-methylthio-2H-1,4-benzothiazine

HRID 434765ノート

反応式

HRID 434765 の反応式
[H-].[Na+].[S:3]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[S:13])[CH2:4]1.[CH3:14]I>CN(C)C=O>[CH3:14][S:13][C:5]1[CH2:4][S:3][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 7739812H-1,4-Benzothiazine-3(4H)-thione

生成物 1

HCID 125454293-methylthio-2H-1,4-benzothiazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In a one liter flask is placed 10.8 parts of prewashed sodium hydride in 150 parts of N,N-dimethyl-formamide (DMF) at room temperature. After stirring for five minutes under nitrogen atmosphere, 30 parts of 2H-1,4-benzothiazine-3(4H)-thione[J. Med. Chem., 12, 290(1969)] is added in portions over a period of 30 minutes and continuously stirred at room temperature for 20 minutes. To the reaction mixture is then added 15 parts of methyl iodide and the mixture stirred at room temperature for 20 minutes under nitrogen. Removal of solvent by vacuum distillation under nitrogen affords 3-methylthio-2H-1,4-benzothiazine as the residue. Since the product is subject to spontaneous hydrolytic decomposition, it is not usually isolated for the purposes of this invention but instead employed as the solution in DMF preparable via the foregoing procedure.

後処理

  1. customIn a one liter flask is placed
  2. customat room temperature
  3. stirringcontinuously stirred at room temperature for 20 minutes
  4. stirringthe mixture stirred at room temperature for 20 minutes under nitrogen
  5. customRemoval of solvent
  6. distillationby vacuum distillation under nitrogen

出典と根拠

ORDレコード
ord-bdc6ff1586e144fa83a26086d1b24a7f
出典データセット
uspto-grants-1983_08
特許番号
US04399279

反応ノート

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