1,1-Dichloroethane → 2,4-Dichlorobenzonitrile
반응식
[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]참가 물질
6
실험 절차
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%.
후처리
- filtrationfiltered
- distillationDichloroethane was distilled off from the filtrate
- additionthe residue was added with water
- customto precipitate the crude crystals
- customThe crude crystals were recrystallized
출처 및 근거
- ORD 기록
- ord-402a1150f9fe498699052d6d9e667ac6
- 출처 데이터셋
- uspto-grants-1980_09
- 특허 번호
- US04225534
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