Sodium Hydroxide → Benzophenone, 2,5-diamino-2'-chloro-

HRID 358048ノート

反応式

HRID 358048 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:12])=[O:5].[Sn](Cl)Cl.[OH-].[Na+]>Cl>[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:12])=[O:5]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 748302-Amino-5-nitro-2'-chlorobenzophenone

生成物 1

HCID 521842Benzophenone, 2,5-diamino-2'-chloro-

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

100 g of 2-amino-2'-chloro-5-nitrobenzophenone are suspended in 865 ml of 25% hydrochloric acid and treated portionwise with a total of 269 g of tin (II) chloride. The mixture is stirred at room temperature for 36 hours, then diluted with 0.5 l of an ice/water mixture and adjusted to pH 10 with about 2.17 l of a 28% sodium hydroxide solution. The mixture is extracted with methylene chloride. After evaporation of the solvent, the residue is dissolved in 0.54 l of ether and crystallized at about -20°. There is obtained 2,5-diamino-2'-chlorobenzophenone of melting point 30°-40°.

後処理

  1. extractionThe mixture is extracted with methylene chloride
  2. customAfter evaporation of the solvent
  3. dissolutionthe residue is dissolved in 0.54 l of ether
  4. customcrystallized at about -20°

出典と根拠

ORDレコード
ord-a8f95aeb9d8c4ca687238f9da1bca3e0
出典データセット
uspto-grants-1984_08
特許番号
US04464300

反応ノート

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