Iodine chloride → Methyl 4-amino-5-iodo-2-methoxybenzoate

HRID 630418ノート

反応式

HRID 630418 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.[I:14]Cl>C(O)(=O)C>[NH2:1][C:2]1[C:11]([I:14])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1

参加物

4

反応物 2

HCID 24640Iodine chlorideHCID 168705Methyl 4-amino-o-anisate

生成物 1

HCID 15700587Methyl 4-amino-5-iodo-2-methoxybenzoate収率 88%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution of methyl 4-amino-2-methoxybenzoate (13 g, 0.07 mol) in acetic acid (300 mL) was added dropwise a solution of iodine monochloride (11.5 g, 0.07 mol) in acetic acid (50 mL). The mixture was stirred for 1.5 hours at room temperature. The precipitate was filtered and washed with ether. Then was dissolved with bicarbonate 4% and extracted with ethyl acetate. The organic layer was washed with brine, dried and the solvent was removed under reduced pressure giving the title compound as a white solid (88%), which was used in the next step without further purification.

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with ether
  3. dissolutionThen was dissolved with bicarbonate 4%
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. customdried
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-b0d898fe99ca41dcbd16a289f92af956
出典データセット
uspto-grants-2016_04
特許番号
US09315463B2

反応ノート

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