3-Aminobenzoic Acid → 3-Aminocyclohexanecarboxylic acid

HRID 1352044

반응식

HRID 1352044 반응식
[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

참가 물질

5

반응물 2

HCID 74193-Aminobenzoic AcidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 5448873-Aminocyclohexanecarboxylic acid수율 57.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-7ab88b7a1e8f4f5f8d5791d0539255af
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217728B2

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