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

HRID 1594000노트

반응식

HRID 1594000 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 229287461-Iodo-3-(methoxymethyl)benzene수율 87.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

반응 조건

온도
30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6a5520588f74ce688898db1a417d5d3
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07300939B2

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