3-Aminobenzoic Acid → 3-Aminocyclohexanecarboxylic acid

HRID 1352044

反応式

HRID 1352044 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[H][H]>C(O)C.[Pd]>[NH2:1][CH:2]1[CH2:10][CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3]1

参加物

5

反応物 2

HCID 74193-Aminobenzoic AcidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 5448873-Aminocyclohexanecarboxylic acid収率 57.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 3-aminobenzoic acid (66.12 g, 0.48 mol) and 10% palladium-on-carbon (13.2 g) in 30% aqueous ethanol (1200 mL) was placed in a 4 L stainless steel high-pressure reactor and reduced at 50° C. and 500 psi of hydrogen for 30 h. The mixture was filtered through Celite and the filter cake was washed with ethanol. The solvent was evaporated, boiling ethanol (1 L) was added and the mixture was allowed to stand for 8 days at room temperature. The mixture was filtered and the product was washed with ethanol and then dried in a vacuum oven at 50° C., to give 3-aminocyclohexanecarboxylic acid (39.30 g, 57%) as a white solid.

後処理

  1. customwas placed in a 4 L stainless steel high-pressure reactor
  2. customreduced at 50° C.
  3. filtrationThe mixture was filtered through Celite
  4. washthe filter cake was washed with ethanol
  5. customThe solvent was evaporated
  6. additionwas added
  7. filtrationThe mixture was filtered
  8. washthe product was washed with ethanol
  9. customdried in a vacuum oven at 50° C.

出典と根拠

ORDレコード
ord-7ab88b7a1e8f4f5f8d5791d0539255af
出典データセット
uspto-grants-2007_05
特許番号
US07217728B2

関連ノート

読み込み中…