Acetic Acid → 2-Iodo-4-methoxyphenylamine

HRID 541904

反応式

HRID 541904 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-])=O)=[C:5]([I:12])[CH:4]=1.C(O)(=O)C>CO.O.[Fe]>[I:12][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=[CH:7][C:6]=1[NH2:9]

参加物

6

反応物 2

HCID 176Acetic AcidHCID 27334564-Nitro-3-iodoanisole

生成物 1

HCID 110103362-Iodo-4-methoxyphenylamine収率 90%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

To a suspension of 3-iodo-4-nitrophenyl methyl ether (5.0 g, 0.018 mol) in methanol (50 mL), water (5 mL), and acetic acid (10 mL) was added iron (3.00 g, 0.0538 mol) powder in small quantities. When the addition was completed, the reaction mixture was heated at 70° C. overnight. After filtration, the cake was rinsed with EtOAc. The filtrate was concentrated and the residue was diluted with NaHCO3 (aq) and EtOAc. After layer separation, the organic layer was dried, filtered and concentrated to give the desired product (4.0 g, 90%).

後処理

  1. additionWhen the addition
  2. filtrationAfter filtration
  3. washthe cake was rinsed with EtOAc
  4. concentrationThe filtrate was concentrated
  5. additionthe residue was diluted with NaHCO3 (aq) and EtOAc
  6. customAfter layer separation
  7. customthe organic layer was dried
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-83834a3d830940cea459d854688122b5
出典データセット
uspto-grants-2014_10
特許番号
US08871753B2

関連ノート

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