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Water → 6-Fluoro-N-(2-fluorophenyl)-3-nitro-4-quinolinamine

HRID 1672314
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반응식

HRID 1672314 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([F:12])[CH:10]=2)[N:5]=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[F:16][C:17]1[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=1[NH2:19].O>C(O)(=O)C>[F:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][C:3]([N+:13]([O-:15])=[O:14])=[C:2]2[NH:19][C:18]1[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=1[F:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 95842-FluoroanilineHCID 108231514-Chloro-6-fluoro-3-nitro-quinoline

생성물 1

HCID 600469356-Fluoro-N-(2-fluorophenyl)-3-nitro-4-quinolinamine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

0.4 g (1.8 mmol) of 4-chloro-6-fluoro-3-nitro-quinoline (Example 19c) and 0.17 ml (1.98 mmol) 2-fluoroaniline in 5 ml acetic acid are stirred overnight at rt. Crystals are formed. The mixture is poured into water, the solid material is filtered off and washed with water. The residue is dissolved in CH2Cl2 and washed twice with water. The organic phase is dried over MgSO4 and most of the solvent is evaporated. The title compound is obtained from this solution as yellow crystals by adding hexane. The compound is filtered off, washed with hexane and dried (70° C., high-vacuum). mp: 161-162° C.; MS: 302 (M++1); HPLC: tret=10.24 min (Grad 1).

후처리

  1. customCrystals are formed
  2. filtrationthe solid material is filtered off
  3. washwashed with water
  4. dissolutionThe residue is dissolved in CH2Cl2
  5. washwashed twice with water
  6. dry with materialThe organic phase is dried over MgSO4 and most of the solvent
  7. customis evaporated

출처 및 근거

ORD 기록
ord-43ed0cb8373a4959ba02acdcfee46b7f
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07998972B2

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