Methyl iodide → 1-Methoxymethyloxy-2,3,4,5-tetramethoxybenzene

HRID 1770240노트

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HRID 1770240 반응식
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([O:13][CH3:14])=[C:7]([O:15][CH3:16])[C:6]=1[OH:17].[C:18](=O)([O-])[O-].[K+].[K+].IC>CN(C=O)C>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([O:13][CH3:14])=[C:7]([O:15][CH3:16])[C:6]=1[O:17][CH3:18]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 200957092-Methoxymethyloxy-4,5,6-trimethoxyphenol

생성물 1

HCID 134955321-Methoxymethyloxy-2,3,4,5-tetramethoxybenzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
45 °C

실험 절차

11.5 g of 2-methoxymethyloxy-4,5,6-trimethoxyphenol prepared in Referential Example 12 and 23.0 g of potassium carbonate were suspended in 100 ml of DMF. The suspension was heated at 45° C. while stirring, and 5.2 ml of iodomethane was dropwise added thereto. After the completion of the dropwise addition, the mixture was heated for 30 min, cooled and separated by filtration. 1 l of water was added to the mother liquor, and the mixture was extracted with ethyl acetate. The organic phase was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=85:15) to prepare 6.2 g of the product compound as a colorless oleaginous substance.

후처리

  1. additionAfter the completion of the dropwise addition
  2. temperaturethe mixture was heated for 30 min
  3. temperaturecooled
  4. customseparated by filtration
  5. addition1 l of water was added to the mother liquor
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe organic phase was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off
  10. customThe residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=85:15)
  11. customto prepare 6.2 g of the product compound as a colorless oleaginous substance

출처 및 근거

ORD 기록
ord-24137d98f4654c7cac6e5c6e711c87c9
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05385942

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