4-Fluoro-2-nitroaniline → HCID 21093461, 화합물

HRID 131325

반응식

HRID 131325 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.F[C:13]1[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:14]=1[C:15]#[N:16].O.[OH-].[Li+]>CS(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:13]2[CH:20]=[CH:19][C:18]([C:21]([F:22])([F:24])[F:23])=[CH:17][C:14]=2[C:15]#[N:16])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1

참가 물질

5

반응물 3

HCID 677694-Fluoro-2-nitroanilineHCID 168937Lithium hydroxide, monohydrateHCID 5210162-Fluoro-5-(trifluoromethyl)benzonitrile

생성물 1

HCID 21093461HCID 21093461, 화합물수율 96%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
70 °C

실험 절차

Combine 4-fluoro-2-nitro-phenylamine (5.0 g, 32.03 mmol), 2-fluoro-5-trifluoromethyl-benzonitrile (6.07 g, 32.03 mmol) and lithium hydroxide monohydrate (4.03 g, 96.08 mmol) in methyl sulfoxide (DMSO, 60 ml). Heat the resulting mixture to 70° C. for 16 hours. Cool the reaction mixture to ambient temperature, then pour into approximately 400 ml of ice water and stir for one hour. Filter the resulting mixture and collect the precipitate to obtain 9.995 g of the title compound (30.73 mmol, 96% yield) as an orange amorphous solid. Product used as is with no further purification: Mass Spectrum (m/e): 326(M+1).

후처리

  1. temperatureCool the reaction mixture to ambient temperature
  2. filtrationFilter the resulting mixture
  3. customcollect the precipitate

출처 및 근거

ORD 기록
ord-709a5f8e5dfe4658858302fdd37086d6
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07384934B2

연결된 노트

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