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

HRID 4281노트

반응식

HRID 4281 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 11246Silver acetate촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-986aa5b3e849477ab861a73561ebea06
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725602

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