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Methyl iodide → N-(4-Methoxy-2-methyl-phenyl)-N-methyl-methanesulfonamide

HRID 1244039
ノート
印刷プレビュー

反応式

HRID 1244039 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][S:10]([CH3:13])(=[O:12])=[O:11])=[C:5]([CH3:14])[CH:4]=1.[H-].[Na+].[CH3:17]I>CN(C=O)C.Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]([CH3:17])[S:10]([CH3:13])(=[O:12])=[O:11])=[C:5]([CH3:14])[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodide2 回HCID 24758Sodium hydrideHCID 15851883N-(4-methoxy-2-methylphenyl)methanesulfonamide

生成物 1

HCID 21931865N-(4-Methoxy-2-methyl-phenyl)-N-methyl-methanesulfonamide

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide
溶媒

実験手順

To a solution of 860 mg (4.0 mmol) N-(4-methoxy-2-methyl-phenyl)-methanesulfonamide in 15 ml DMF at ambient temperature was added 192 mg (48 mmol) 60% sodium hydride dispersion and the resulting mixture was treated with 1.14 gm, 0.5 ml (8.0 mmol) methyl iodide. The reaction mixture was stirred at room temperature for 2 hours and 0.5 ml of methyl iodide was introduced and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with 1N HCl and then extracted with ethyl acetate. The organics were washed with brine, dried with sodium sulfate and then evaporated in vacuo to afford 293 mg (X %) of a light purple solid. Mass spectrum APCI (m/z) 230 (p+1).

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 16 hours
  2. extractionextracted with ethyl acetate
  3. washThe organics were washed with brine
  4. dry with materialdried with sodium sulfate
  5. customevaporated in vacuo
  6. customto afford 293 mg (X %) of a light purple solid

出典と根拠

ORDレコード
ord-d8150dc647fd4e398604cdb269f3f0a1
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07119207B2

反応ノート

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