Stannous Chloride → HCID 20088007、化合物

HRID 275368ノート

反応式

HRID 275368 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[C:6]([CH:8]=1)[NH2:7].[N:18]([O-])=O.[Na+].Cl[Sn]Cl>Cl.O>[Cl:1][C:2]1[CH:8]=[C:6]2[C:5]([C:9]([C:10]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=3)=[N:18][NH:7]2)=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 24479Stannous ChlorideHCID 223994925-chloro-2-(4-fluorobenzoyl)anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 20088007HCID 20088007、化合物収率 50.6%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

実験手順

To solution of 5-chloro-2-(4-fluorobenzoyl)aniline (5 g) in 6M aqueous HCl (25 ml) was added a solution of NaNO2 (2.5 g) in water (5 ml) at 0°-5° C. under stirring during 15 min. After stirring for further 0.5 h at 0° C. a solution of SnCl2 (20 g) in conc. aqueous HCl (25 ml) was added. The reaction mixture was allowed to heat to room temperature and after 0.5 h the precipitate was filtered off and suspended in 2 N aqueous NaOH. The suspension was filtered and dichloromethane was added to the precipitate. The thus obtained solution was washed with brine and dried (MgSO4). Evaporation of the solvents afforded the title compound (2.5 g) as an oil which was used without further purification. In a corresponding manner the following indazole derivative was prepared: 3-(4-Fluorophenyl)-5-trifluoromethyl-1H-indazole 25b, (oil)

後処理

  1. additionwas added
  2. filtrationwas filtered off
  3. filtrationThe suspension was filtered
  4. additiondichloromethane was added to the precipitate
  5. washThe thus obtained solution was washed with brine
  6. dry with materialdried (MgSO4)
  7. customEvaporation of the solvents

出典と根拠

ORDレコード
ord-1913f0cdb15f4a8f8f75847c3fae3d06
出典データセット
uspto-grants-1995_02
特許番号
US05393761

反応ノート

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