Methanol → 3-Methoxy-1,2,4,5-tetramethylbenzene

HRID 1164285

反応式

HRID 1164285 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[C:4]([CH3:10])[C:3]=1[OH:11].[CH3:12]I.[H-].[Na+].CO>CS(C)=O.CCOCC.O>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[C:4]([CH3:10])[C:3]=1[O:11][CH3:12]

参加物

8

反応物 4

HCID 887MethanolHCID 6328Methyl iodideHCID 106942,3,5,6-TetramethylphenolHCID 24758Sodium hydride2 回

生成物 1

HCID 2786643-Methoxy-1,2,4,5-tetramethylbenzene

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

In 150 ml of DMSO were dissolved 15.0 g of 2,3,5,6-tetramethylphenol and 28 ml of methyl iodide. Under ice-cooling 6.3 g of 60% sodium hydride in oil was added, and the mixture was stirred at room temperature for 1 hour. The excess sodium hydride was decomposed with MeOH and after addition of water extraction with ether was carried out. The extract was dried over sodium sulfate. Removal of the solvent by distillation leaves crystals which were recrystallized from MeOH.

後処理

  1. additionwas added
  2. dry with materialThe extract was dried over sodium sulfate
  3. customRemoval of the solvent
  4. distillationby distillation
  5. customleaves crystals which
  6. customwere recrystallized from MeOH

出典と根拠

ORDレコード
ord-655501f6e8924ea0b35aba1e4c8912f1
出典データセット
uspto-grants-1983_01
特許番号
US04368150

関連ノート

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