Ammonia → 4-(1-Aminoethyl)benzoic acid

HRID 622408

反応式

HRID 622408 の反応式
[C:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)(=O)[CH3:2].[NH3:13]>[Ni]>[NH2:13][CH:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)[CH3:2]

参加物

4

反応物 2

HCID 222AmmoniaHCID 114704-Acetylbenzoic Acid

生成物 1

HCID 125682714-(1-Aminoethyl)benzoic acid

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

4-Acetylbenzoic acid (4.1 g) is dissolved in 50 mL ammonia-saturated methanol. Raney nickel catalyst (1.5 g; activity grade III) is then added and the mixture reduced under hydrogen atmosphere (4750 psi) at 80° C. for 17 hrs. After removal of the catalyst by suction filtration, the filtrate is evaporated and the residue dissolved in H2O. The solution is passed through a 2.5×15 cm column of Dowex 50X8-400 resin (H+ form) and eluted with 1N NH4OH. Evaporation of the eluate leaves a residue (2.9 g) which is recrystallized from H2O/acetone and characterized as 4-(1-aminoethyl)benzoic acid, m.p.>300° C.

後処理

  1. customat 80° C.
  2. customfor 17 hrs
  3. customAfter removal of the catalyst
  4. filtrationby suction filtration
  5. customthe filtrate is evaporated
  6. dissolutionthe residue dissolved in H2O
  7. washeluted with 1N NH4OH
  8. customEvaporation of the eluate

出典と根拠

ORDレコード
ord-22eabd9128c64e8e8810484ca096656c
出典データセット
uspto-grants-1988_09
特許番号
US04771064

関連ノート

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