Acetic Acid → Mls000756290

HRID 461296ノート

反応式

HRID 461296 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[NH:13][CH2:14][CH3:15])[C:7]([NH2:9])=[O:8])([O-])=O.[C:16](OC(=O)C)(=O)[CH3:17].C(O)(=O)C>[Ni]>[CH2:14]([N:13]1[C:12]2[CH:11]=[CH:10][C:6]([C:7](=[O:8])[NH2:9])=[CH:5][C:4]=2[N:1]=[C:16]1[CH3:17])[CH3:15]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 37089224-Ethylamino-3-nitrobenzamide

生成物 1

HCID 292579Mls000756290収率 88%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

A mixture of 125 g (0.6 mole) of compound III, 214 g (2.1 moles) of acetic anhydride, 1.2 ml of Raney nickel and 36 g (0.6 mole) of acetic acid was hydrogenated at 80° C and a pressure of 100 to 30 kg/sq.cm for 5 h. After cooling, the catalyst was filtered, and the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. Then 150 ml of 6N sulphuric acid were added to the residue. The reaction was very exothermic. The solution was refluxed with active carbon for 15 min and filtered. The filtrate was mixed with 1.2 kg of ice and exactly neutralized with 2N sodium hydroxide. The precipitate was washed with water and dried at 100° C. Melting point: 251° C. Yield: 88% (108 g).

後処理

  1. customwas hydrogenated at 80° C
  2. temperatureAfter cooling
  3. filtrationthe catalyst was filtered
  4. concentrationthe filtrate was concentrated by normal pressure until 135 ml of distillate
  5. customwere collected
  6. additionThen 150 ml of 6N sulphuric acid were added to the residue
  7. temperatureThe solution was refluxed with active carbon for 15 min
  8. filtrationfiltered
  9. additionThe filtrate was mixed with 1.2 kg of ice
  10. washThe precipitate was washed with water
  11. customdried at 100° C

出典と根拠

ORDレコード
ord-8053dfd953ee47138cdbee4d00589cb3
出典データセット
uspto-grants-1977_12
特許番号
US04062682

反応ノート

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