Dimethylformamide → 4-Chloro-2-nitrobenzonitrile

HRID 370635

反応式

HRID 370635 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[Cu][C:13]#[N:14].CN(C)C=O.C(OCC)(=O)C>>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]([C:13]#[N:14])=[C:3]([N+:9]([O-:11])=[O:10])[CH:4]=1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 69772,5-DichloronitrobenzeneHCID 8857Ethyl AcetateHCID 178418546HCID 178418546、化合物

生成物 1

HCID 969244-Chloro-2-nitrobenzonitrile収率 63%

実験手順

A mixture of 7.7 g (0.040 mol) of 2,5-dichloronitrobenzene and 4.0 g (0.044 mol) of copper (I) cyanide in 4.0 ml (0.05 mol) of N,N-dimethylformamide was refluxed for 3.5 hours. The reaction mixture was poured slowly into 39 ml (0.40 mol) of ethyl acetate and followed by stirring for 10 hours at room temperature. The precipitate was filtered and washed with 3 ml of ethyl acetate. After concentration of the combined filtrate, the residue gave 4.6 g (63.0%) of 4-chloro-2-nitrobenzonitrile purified by the procedure of Example 1.

後処理

  1. temperaturewas refluxed for 3.5 hours
  2. filtrationThe precipitate was filtered
  3. washwashed with 3 ml of ethyl acetate

出典と根拠

ORDレコード
ord-92feba178098441aa1eabb90f9bbe19e
出典データセット
uspto-grants-1985_07
特許番号
US04528143

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