Iodine → 4-(2-Iodo-5-methoxyphenyl)butan-2-one

HRID 4281

反応式

HRID 4281 の反応式
[I:1]I.[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13](=[O:15])[CH3:14])[CH:8]=[CH:9][CH:10]=1>C(O)(=O)C.C([O-])(=O)C.[Ag+]>[I:1][C:8]1[CH:9]=[CH:10][C:5]([O:4][CH3:3])=[CH:6][C:7]=1[CH2:11][CH2:12][C:13](=[O:15])[CH3:14]

参加物

5

反応物 2

HCID 807IodineHCID 114239024-(3-Methoxyphenyl)butan-2-one

生成物 1

HCID 140254744-(2-Iodo-5-methoxyphenyl)butan-2-one収率 82.3%

試薬・触媒・溶媒 2

HCID 11246Silver acetate触媒HCID 176Acetic Acid溶媒

実験手順

Samples of iodine (42.4 g, 0.167 mole) and silver acetate (27.87 g, 0.167 mole) were added in portions to a solution of 29.8 g (0.167 mole) of 1-(3-methoxyphenyl)butane-3-one in 167 ml of glacial acetic acid. The mixture was stirred one hour. The silver iodide was removed by filtration and washed with acetic acid. The filtrate was partitioned between ether and water. The ether layer was washed with water, sodium bicarbonate solution and sodium thiosulfate solution. The ether solution was dried with MgSO4 and evaporated to dryness in vacuo. There was obtained 41.8 g (82% yield) of oily 1-(2-iodo-5-methoxyphenyl)butane-3-one.

後処理

  1. customThe silver iodide was removed by filtration
  2. washwashed with acetic acid
  3. customThe filtrate was partitioned between ether and water
  4. washThe ether layer was washed with water, sodium bicarbonate solution and sodium thiosulfate solution
  5. dry with materialThe ether solution was dried with MgSO4
  6. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-986aa5b3e849477ab861a73561ebea06
出典データセット
uspto-grants-1988_02
特許番号
US04725602

関連ノート

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