1,1-Dichloroethane → 2,4-Dichlorobenzonitrile

HRID 28092

反応式

HRID 28092 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+]([O-])=O)[CH:3]=1.[Cl-].[Li+].[Cl-].[Al+3].[Cl-].[Cl-].[Cl:19]C(Cl)C>CN1CCCC1=O>[Cl:19][C:4]1[CH:3]=[C:2]([Cl:1])[CH:9]=[CH:8][C:5]=1[C:6]#[N:7]

参加物

6

反応物 4

HCID 63651,1-DichloroethaneHCID 969244-Chloro-2-nitrobenzonitrileHCID 433294Lithium ChlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 810502,4-Dichlorobenzonitrile収率 79.2%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

4.55 parts of 4-chloro-2-nitrobenzonitrile, 0.42 parts of lithium chloride, 1.11 parts of anhydrous aluminum chloride and 15 parts of N-methyl-2-pyrrolidone were reacted at 180° C. for 3 hours after the pattern of EXAMPLE B1. The reaction solution was added with 100 parts of dichloroethane, agitated for 30 minutes and filtered. Dichloroethane was distilled off from the filtrate and the residue was added with water to precipitate the crude crystals. The crude crystals were recrystallized by using a water-methanol mixed solvent to obtain 3.4 parts of 2,4-dichlorobenzonitrile with purity of 99%. Yield: 79.2%.

後処理

  1. filtrationfiltered
  2. distillationDichloroethane was distilled off from the filtrate
  3. additionthe residue was added with water
  4. customto precipitate the crude crystals
  5. customThe crude crystals were recrystallized

出典と根拠

ORDレコード
ord-402a1150f9fe498699052d6d9e667ac6
出典データセット
uspto-grants-1980_09
特許番号
US04225534

関連ノート

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