4-Chloroaniline → HCID 178449876, 화합물

HRID 75484노트

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HRID 75484 반응식
[C:1](#[N:5])[CH2:2][CH2:3][CH3:4].[Al+3].[Cl-].[Cl-].[Cl-].[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1>C1(C)C=CC=CC=1.O>[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH:15][C:1](=[NH:5])[CH2:2][CH2:3][CH3:4])=[CH:13][CH:12]=1

참가 물질

6

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온도
115 °C

실험 절차

To a solution of butyronitrile (compound 2, 7.5 mL, 86.2 mmol), AlCl3 in toluene was added 4-chloroaniline (compound 1, 10.0 g, 78.4 mmol). The reaction mixture was stirred at 115° C. for 5 hrs. The mixture was diluted with water (200 mL) and extracted with EtOAc (200 mL) The aqueous layer was neutralized with saturated NaHCO3 (500 mL) and extracted with EtOAc (300 mL×2). The organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The obtained product (9.2 g, pale brown solid) was used for the next step without purification.

후처리

  1. extractionextracted with EtOAc (200 mL) The aqueous layer
  2. extractionextracted with EtOAc (300 mL×2)
  3. dry with materialThe organic layer was dried over anhydrous MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe obtained product (9.2 g, pale brown solid) was used for the next step without purification

출처 및 근거

ORD 기록
ord-5d9fdc9310e449abab4ec5622bb74e20
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835436B2

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