Dimethylformamide → 4-Chloro-2-nitrobenzonitrile

HRID 370635

반응식

HRID 370635 반응식
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

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 69772,5-DichloronitrobenzeneHCID 8857Ethyl AcetateHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 969244-Chloro-2-nitrobenzonitrile수율 63%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-92feba178098441aa1eabb90f9bbe19e
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528143

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