2,5-Difluoronitrobenzene → 2-(4-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile

HRID 1350499

반응식

HRID 1350499 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([CH:10]([CH3:12])[CH3:11])=[CH:6][C:3]=1[C:4]#[N:5].F[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[N+:21]([O-:23])=[O:22].O.[OH-].[Li+]>CS(C)=O>[F:20][C:17]1[CH:18]=[CH:19][C:14]([NH:1][C:2]2[CH:9]=[CH:8][C:7]([CH:10]([CH3:12])[CH3:11])=[CH:6][C:3]=2[C:4]#[N:5])=[C:15]([N+:21]([O-:23])=[O:22])[CH:16]=1

참가 물질

5

반응물 3

HCID 677672,5-DifluoronitrobenzeneHCID 168937Lithium hydroxide, monohydrateHCID 210934632-Amino-5-isopropylbenzonitrile

생성물 1

HCID 210934592-(4-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile수율 81%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Heat a solution of 2-amino-5-isopropyl-benzonitrile (1.482 g, 9.25 mmol) with 1,4-difluoro-2-nitro-benzene (1.47 g, 9.25 mmol) and lithium hydroxide monohydrate (0.78 g, 18.50 mmol) in DMSO (20 ml) to 70° C. for 38 hours. Cool the reaction to ambient temperature and then pour into approximately 200 ml of ice water and stir for one hour. The title compound precipitates and collection by filtration to obtain 2.236 g (7.47 mmol, 81% yield) of the title compound as an orange amorphous solid: Mass Spectrum (m/e): 300(M+1).

후처리

  1. temperatureCool
  2. customthe reaction to ambient temperature
  3. customThe title compound precipitates
  4. customcollection
  5. filtrationby filtration

출처 및 근거

ORD 기록
ord-27640c6639d946e1b1e949c2d6d8860a
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214673B2

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