Ethanol → 4-AMINO-N-THIAZOL-2-YL-BENZAMIDE

HRID 2243434노트

반응식

HRID 2243434 반응식
[N+:1]([C:4]1[CH:17]=[CH:16][C:7]([C:8]([NH:10][C:11]2[S:12][CH:13]=[CH:14][N:15]=2)=[O:9])=[CH:6][CH:5]=1)([O-])=O.CCO.C(OCC)(=O)C>[Pd].C(O)(=O)C>[NH2:1][C:4]1[CH:17]=[CH:16][C:7]([C:8]([NH:10][C:11]2[S:12][CH:13]=[CH:14][N:15]=2)=[O:9])=[CH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 702EthanolHCID 8857Ethyl AcetateHCID 2303634-Nitro-N-(1,3-thiazol-2-yl)benzamide

생성물 1

HCID 2254704-AMINO-N-THIAZOL-2-YL-BENZAMIDE

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

4-Nitro-N-thiazol-2-yl-benzamide (28 mmol) was suspended in abs. EtOH (400 mL) and ethyl acetate (200 mL) and glacial acetic acid (50 mL) was added followed by 10% Pd/C (0.5 g). The mixture was hydrogenated for 72 h at 3 bar H2. The hydrogenation mixture was filtered, and the solvent was removed under reduced pressure. The crude product was added NaHCO3 (sat.) and ethyl acetate, the remaining solid fraction was removed by filtration and dried in vacuo. The liquid phases were separated, the organics were washed with brine, dried over MgSO4, filtered and evaporated to yield a solid. The solid fractions were combined.

후처리

  1. filtrationThe hydrogenation mixture was filtered
  2. customthe solvent was removed under reduced pressure
  3. additionThe crude product was added NaHCO3 (sat.) and ethyl acetate
  4. customthe remaining solid fraction was removed by filtration
  5. customdried in vacuo
  6. customThe liquid phases were separated
  7. washthe organics were washed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated
  11. customto yield a solid

출처 및 근거

ORD 기록
ord-9a61c3e0078b4a8a971519cfc66ed2a0
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674912B2

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