Methyl iodide → 1-Iodo-3-(methoxymethyl)benzene

HRID 1594000ノート

反応式

HRID 1594000 の反応式
[I:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].IC.[C:12](=O)([O-])[O-].[K+].[K+].[H-].[Na+]>CC#N.O>[CH3:12][O:6][CH2:5][C:4]1[CH:3]=[C:2]([I:1])[CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 423003-Iodobenzyl alcohol

生成物 1

HCID 229287461-Iodo-3-(methoxymethyl)benzene収率 87.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
30 °C

実験手順

To a solution of 508 μl (4.0 mmol) of 3-iodobenzylalcohol and 1.25 ml (20.0 mmol) of iodomethane in MeCN (20 ml) there were added 829 mg (6.0 mmol) of potassium carbonate. After stirring 3 h at 30° C., 320 mg (8.00 mmol) of NaH were added and stirring was continued a further 3 h at RT. Water was then added to the reaction mixture, which was extracted with chloroform. The organic phase was successively washed with water and a satd aq. NaCl soln and dried over MgSO4. Following filtration and removal of the solvent in vacuo there were obtained 863 mg (3.5 mmol, 87%) of 3-methoxymethyliodobenzene.

後処理

  1. stirringstirring
  2. waitwas continued a further 3 h at RT
  3. extractionwas extracted with chloroform
  4. washThe organic phase was successively washed with water
  5. dry with materiala satd aq. NaCl soln and dried over MgSO4
  6. filtrationfiltration and removal of the solvent in vacuo

出典と根拠

ORDレコード
ord-c6a5520588f74ce688898db1a417d5d3
出典データセット
uspto-grants-2007_11
特許番号
US07300939B2

反応ノート

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