Iodine → 2-Iodo-4-methyl-6-nitroaniline

HRID 1466474

반응식

HRID 1466474 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[I:12]I>C(O)C.[N+]([O-])([O-])=O.[Ag+]>[NH2:8][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]([CH3:1])=[CH:7][C:6]=1[I:12]

참가 물질

5

반응물 2

HCID 807IodineHCID 69784-Methyl-2-nitroaniline

생성물 1

HCID 197351992-Iodo-4-methyl-6-nitroaniline수율 79.3%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 702Ethanol용매

실험 절차

Commercially available 4-methyl-2-nitro-phenylamine (20 g, 131.5 mmol) was dissolved in ethanol (300 mL), silver nitrate (27 g, 157.7 mmol) and iodine (40 g, 157.7 mmol) were added thereto, and the mixture was stirred for 8 h at room temperature. After completion of the reaction, the reaction mixture was filtered through a cellite, washed with 100 mL of ethyl acetate, and concentrated. Water was added to the residue, which was then extracted with ethyl acetate, washed with saturated sodium chloride solution, and dried over anhydrous magnesium sulfate to give the title compound (29 g, Yield 69%).

후처리

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture was filtered through a cellite
  3. washwashed with 100 mL of ethyl acetate
  4. concentrationconcentrated
  5. additionWater was added to the residue, which
  6. extractionwas then extracted with ethyl acetate
  7. washwashed with saturated sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-d64dc385be1249189cd881876e7fb1df
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000028B2

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