4-Chloroaniline → HCID 178449876、化合物

HRID 75484ノート

反応式

HRID 75484 の反応式
[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

参加物

6

反応物 3

HCID 78124-Chloroaniline2 回HCID 8008Butyronitrile2 回HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 178449876HCID 178449876、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

反応条件

温度
115 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5d9fdc9310e449abab4ec5622bb74e20
出典データセット
uspto-grants-2014_09
特許番号
US08835436B2

反応ノート

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