Acetic Acid → 3-Chloro-4-(3-chlorophenoxy)aniline

HRID 38242

反応式

HRID 38242 の反応式
C(O)(=O)C.[Cl:5][C:6]1[CH:11]=[C:10]([N+:12]([O-])=O)[CH:9]=[CH:8][C:7]=1[O:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=1>O.CCO.[Fe]>[Cl:5][C:6]1[CH:11]=[C:10]([CH:9]=[CH:8][C:7]=1[O:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=1)[NH2:12]

参加物

5

反応物 2

HCID 176Acetic AcidHCID 2752072-Chloro-1-(3-chlorophenoxy)-4-nitrobenzene

生成物 1

HCID 176055343-Chloro-4-(3-chlorophenoxy)aniline収率 100%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 19096565Water ethanol溶媒

実験手順

According to Scheme 3 Step 2: A suspension of iron (5.07 mmol, 283 mg), acetic acid (1.22 mmol, 70 μL) and of 2-chloro-1-(3-chlorophenoxy)-4-nitrobenzene (1.02 mmol, 288 mg) in water/EtOH (1:1, 8 mL) was stirred at 80° C. for 30 minutes. After evaporation of EtOH, the aqueous phase was basified with a saturated solution of NaHCO3 and was extracted with AcOEt. The organic phase was washed with brine, was dried over MgSO4, was filtered and was concentrated under reduced pressure to yield 3-chloro-4-(3-chlorophenoxy)aniline (1.02 mmol, 258 mg, 100%) as a solid. The product was used without further purification.

後処理

  1. customAfter evaporation of EtOH
  2. extractionwas extracted with AcOEt
  3. washThe organic phase was washed with brine
  4. dry with materialwas dried over MgSO4
  5. filtrationwas filtered
  6. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-077c9c4ea8274fb796a20617fa6ba2d7
出典データセット
uspto-grants-2013_09
特許番号
US08524726B2

関連ノート

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