Iodine → Methyl 4-amino-3-iodobenzoate

HRID 11415

反応式

HRID 11415 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.[I:12]I>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:11]=1[I:12]

参加物

5

反応物 2

HCID 807IodineHCID 12082Methyl 4-aminobenzoate

生成物 1

HCID 4104649Methyl 4-amino-3-iodobenzoate

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

Methyl 4-aminobenzoate (30.23 g, 200 mmol) was added to a mixture of iodine (60.91 g, 240 mmol) and silver sulfate (81.07 g, 260 mmol) in 1 L of ethanol at room temperature. The mixture was stirred at room temperature for 18 hours, filtered over Celite and the filtrate was evaporated to dryness under reduced pressure. The residue was chromatographed on silica gel (230–400 mesh) and eluted with 1% ethyl acetate in hexane to give 35 g (63%).

後処理

  1. filtrationfiltered over Celite
  2. customthe filtrate was evaporated to dryness under reduced pressure
  3. customThe residue was chromatographed on silica gel (230–400 mesh)
  4. washeluted with 1% ethyl acetate in hexane
  5. customto give 35 g (63%)

出典と根拠

ORDレコード
ord-f7ee27120d3e45df9a00b6188ab0a4c8
出典データセット
uspto-grants-2006_08
特許番号
US07098231B2

関連ノート

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