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

HRID 1672314
ノート
印刷プレビュー

反応式

HRID 1672314 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-43ed0cb8373a4959ba02acdcfee46b7f
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07998972B2

反応ノート

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