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

HRID 1164285

반응식

HRID 1164285 반응식
[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]

참가 물질

8

반응물 4

HCID 887MethanolHCID 6328Methyl iodideHCID 106942,3,5,6-TetramethylphenolHCID 24758Sodium hydride2회

생성물 1

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

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-655501f6e8924ea0b35aba1e4c8912f1
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04368150

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