Sodium Carbonate → 3,3'-Diaminobenzophenone

HRID 637557

反応式

HRID 637557 の反応式
Cl[C:2]1[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9](F)=[C:8]([N+:13]([O-])=O)[CH:7]=1)=[O:5].C(=O)([O-])[O-].[Na+].[Na+].[H][H]>[Pd].C(O)C>[NH2:13][C:8]1[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=1)[C:4]([C:3]1[CH:2]=[CH:19][CH:18]=[C:17]([NH2:20])[CH:16]=1)=[O:5]

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 202571122-Chloro-4'-fluoro-5,3'-dinitro benzophenoneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 691453,3'-Diaminobenzophenone

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

In an autoclave there are added 32.5 g (0.1 moles) of 2-chloro-4'-fluoro-5,3'-dinitro benzophenone, 15.9 g (0.15 moles) of sodium carbonate, 2 g of 5% palladium/alumina catalyst (from Nihon-Engelhardt Co.) and 100 ml of ethanol. With the mixture being stirred at 30°-35° C., there is introduced hydrogen into the autoclave, at a constant pressure of 10 Kg/cm2. G, to carry out the reaction for ten hours. After the completion of the reaction, the reaction mixture is heated up to filter out the catalyst and the inorganic salt. Then, on cooling the mixture there is obtained 3,3'-diamino benzophenone in the form of yellow needle-like crystals. The crystals are filtered, washed with 10 ml of ethanol and dried. Yield 16.2 g (76.3%). M.P. 149°-151° C.

後処理

  1. customthe reaction for ten hours
  2. customAfter the completion of the reaction
  3. temperaturethe reaction mixture is heated up
  4. filtrationto filter out the catalyst
  5. temperatureThen, on cooling the mixture there

出典と根拠

ORDレコード
ord-427fbe334cca4260af1426e7f16c5a62
出典データセット
uspto-grants-1985_12
特許番号
US04556738

関連ノート

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