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Isopropylamine → N-Isopropyl-2-nitroaniline

HRID 334731
ノート
印刷プレビュー

反応式

HRID 334731 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH:11]([NH2:14])([CH3:13])[CH3:12]>CCO>[CH:11]([NH:14][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])([CH3:13])[CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6363Isopropylamine3 回HCID 738951-Fluoro-2-nitrobenzene

生成物 1

HCID 10583518N-Isopropyl-2-nitroaniline収率 93.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1-fluoro-2-nitrobenzene (4.406 g, 31.22 mmol) in EtOH (32 mL) was added at 0° C. isopropyl amine (2.97 mL, 32.80 mmol). The mixture turned from light yellow to bright orange instantly. It was stirred overnight at RT. Another 1 eq of isopropyl amine (2.97 mL, 32.80 mmol) was added and after 3 h of stirring 2 eq of isopropyl amine were added (6 mL, 64 mmol) and the resulting solution was kept at room temperature overnight. The reaction mixture was concentrated and another equivalent of isopropyl amine was added (2.97 mL) following by EtOH (2 mL). For completion, the reaction was heated at 50° C. for 2 h. Mixture was evaporated to dryness and dissolved in EtOAc (25 mL) and the organic phase was washed with water (3*10 mL). Aqueous phase was re-extracted with EtOAc (10 mL) and the combined organics were washed with brine and dried over Na2SO4. The solvent was evaporated under reduced pressure to afford 5.24 g of N-isopropyl-2-nitrobenzenamine (Yield: 93%) as an orange liquid

後処理

  1. additionwere added (6 mL, 64 mmol)
  2. waitthe resulting solution was kept at room temperature overnight
  3. concentrationThe reaction mixture was concentrated
  4. additionanother equivalent of isopropyl amine was added (2.97 mL)
  5. temperatureFor completion, the reaction was heated at 50° C. for 2 h
  6. customMixture was evaporated to dryness
  7. dissolutiondissolved in EtOAc (25 mL)
  8. washthe organic phase was washed with water (3*10 mL)
  9. extractionAqueous phase was re-extracted with EtOAc (10 mL)
  10. washthe combined organics were washed with brine
  11. dry with materialdried over Na2SO4
  12. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-83bee91e214d43628566341074a18795
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883826B2

反応ノート

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