Methyl iodide → HCID 19926461、化合物

HRID 1647165ノート

反応式

HRID 1647165 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 19926461HCID 19926461、化合物収率 20.6%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9cc9654cd47f495994330c1bdeb041e4
出典データセット
uspto-grants-1995_07
特許番号
US05430042

反応ノート

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