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Sodium Hydroxide → HCID 19779367、化合物

HRID 1461731
ノート
印刷プレビュー

反応式

HRID 1461731 の反応式
[Cl:1][C:2]1[C:3]([F:15])=[C:4]([N+:12]([O-])=O)[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[OH-].[Na+]>Cl>[NH2:12][C:4]1[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=[C:2]([Cl:1])[C:3]=1[F:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 27365653-Chloro-4-fluoro-5-nitrobenzotrifluoride

生成物 1

HCID 19779367HCID 19779367、化合物収率 73%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

5-Chloro-4-fluoro-3-nitrotrifluoromethylbenzene (50 g) was added to a cooled (5° C.) solution of stannous chloride (140 g) in concentrated agueous hydrochloric acid (187 ml). After stirring for several hours at the ambient temperature (ca 22° C.), the reaction mixture was stood overnight. After basification by the addition of sodium hydroxide, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried, and the solvent removed by evaporation under reduced pressure. The residual yellow oil was kugelrohr distilled under reduced pressure to give 3-amino-5-chloro-4-fluorotrifluoromethylbenzene (32 g):bp. 105° C./11 mm Hg; 'H NMR δ (CDCl3) 7.03 (1H, dq), 6.90 (1H, dq).

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. customthe solvent removed by evaporation under reduced pressure
  5. distillationThe residual yellow oil was kugelrohr distilled under reduced pressure

出典と根拠

ORDレコード
ord-775e46c1ff9f4791ae7747f812f3f436
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05077297

反応ノート

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