Methyl iodide → HCID 19926461, 화합물

HRID 1647165노트

반응식

HRID 1647165 반응식
[OH:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[C:11](=[O:12])[CH:10]=[CH:9][O:8][C:7]=1[CH3:13].[OH-].[K+].[CH3:16]I>>[CH3:16][O:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[C:11](=[O:12])[CH:10]=[CH:9][O:8][C:7]=1[CH3:13]

참가 물질

4

반응물 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 104649893-(3-Hydroxypropoxy)-2-methyl-4H-pyran-4-one

생성물 1

HCID 19926461HCID 19926461, 화합물수율 20.6%

실험 절차

A mixture of 3-(3-hydroxy-1-propoxy)-2-methyl-4-pyrone {1.4 g, 7.6 mmol), 85% KOH (0.55 g, 8.4 mmol) and methyliodide (11 g, 76 mmol) was stirred at room temperature for one day. The red solution was partitioned between methylene chloride and half saturated aqueous ammoniumchloride solution. The organic phase was washed with water, dried over Na2SO4 and evaporated. The residue was purified by chromatography on silica gel with methanol/methylene chloride (3:97) as eluent. Removing the eluent by film evaporation afforded 0.31 g (20%) of the desired product as an oil.

후처리

  1. customThe red solution was partitioned between methylene chloride and half saturated aqueous ammoniumchloride solution
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customThe residue was purified by chromatography on silica gel with methanol/methylene chloride (3:97) as eluent
  6. customRemoving the eluent
  7. customby film evaporation

출처 및 근거

ORD 기록
ord-9cc9654cd47f495994330c1bdeb041e4
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05430042

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