Epichlorohydrin → [(2-Iodo-5-methoxyphenoxy)methyl]oxirane

HRID 1906506ノート

反応式

HRID 1906506 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[OH:10].[H-].[Na+].[CH2:13]([CH:15]1[O:17][CH2:16]1)Cl>>[I:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[O:10][CH2:13][CH:15]1[CH2:16][O:17]1

参加物

4

反応物 3

HCID 7835EpichlorohydrinHCID 24758Sodium hydrideHCID 114140152-Iodo-5-methoxyphenol

生成物 1

HCID 20212121[(2-Iodo-5-methoxyphenoxy)methyl]oxirane収率 93%

反応条件

温度
5 °C

実験手順

A 5.0 g (0.02 mole) sample of 2-iodo-5-methoxyphenol was added in portions to a suspension of 1.01 g (0.021 mole) of 50% sodium hydride (from which the oil had been removed by washing with hexane) in 40 ml of dry DMF. The resulting solution was cooled to 5° C. and 9.14 g (0.099 mole) of epichlorohydrin was added. The mixture was heated at 60° C. for 15 minutes. The mixture was cooled and filtered through diatomaceous earth. The solvent was evaporated in vacuo from the filtrate. The residue was taken up in ether, the ether washed with water and brine, dried (MgSO4) and the solvent evaporated in vacuo to give 5.72 g (93% yield) of [(2-iodo-5-methoxyphenoxy)methyl]oxirane as a brown oil.

後処理

  1. customhad been removed
  2. washby washing with hexane) in 40 ml of dry DMF
  3. temperatureThe mixture was heated at 60° C. for 15 minutes
  4. temperatureThe mixture was cooled
  5. filtrationfiltered through diatomaceous earth
  6. customThe solvent was evaporated in vacuo from the filtrate
  7. washthe ether washed with water and brine
  8. dry with materialdried (MgSO4)
  9. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-e4565a4d053b434192bae8bf23f3dfc2
出典データセット
uspto-grants-1987_03
特許番号
US04652584

反応ノート

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