1,1-Dichloroethane → 2,4-Dichlorobenzonitrile
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
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
- filtrationfiltered
- distillationDichloroethane was distilled off from the filtrate
- additionthe residue was added with water
- customto precipitate the crude crystals
- 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
反応ノート
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