4-Fluoroaniline → HCID 60046932、化合物

HRID 1672309ノート

反応式

HRID 1672309 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:12])=[CH:9][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][C:20]([NH2:21])=[CH:19][CH:18]=1>O>[Cl:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([NH:21][C:20]3[CH:22]=[CH:23][C:17]([F:16])=[CH:18][CH:19]=3)=[C:3]([N+:13]([O-:15])=[O:14])[CH:4]=[N:5]2)=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 97314-FluoroanilineHCID 534398754,7-Dichloro-3-nitroquinoline

生成物 1

HCID 60046932HCID 60046932、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.3 g (5.3 mmol) 4,7-dichloro-3-nitro-quinoline (Example 15b) and 0.525 g (5.3 mmol) 4-fluoroaniline are stirred at rt for 1 h. The reaction mixture is poured into 150 ml of water, and the resulting crystals are filtered off. After washing with water, the solid is dissolved in ca. 170 ml of ethanol and then concentrated to ca. 30 ml. The solution is cooled in ice-water. The crystals which precipitate are filtered off and dried overnight at 70° C. (high vacuum). mp: 198-200° C.; MS: 318 (M++1); HPLC: tret=10.92 min (Grad 1).

後処理

  1. filtrationthe resulting crystals are filtered off
  2. washAfter washing with water
  3. dissolutionthe solid is dissolved in ca. 170 ml of ethanol
  4. concentrationconcentrated to ca. 30 ml
  5. temperatureThe solution is cooled in ice-water
  6. filtrationThe crystals which precipitate are filtered off
  7. customdried overnight at 70° C. (high vacuum)
  8. customtret=10.92 min (Grad 1)

出典と根拠

ORDレコード
ord-ace51838c99e490f8f2c6e54d9902c88
出典データセット
uspto-grants-2011_08
特許番号
US07998972B2

反応ノート

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