Sodium Carbonate → 1-(4-Amino-2-fluoro-phenyl)-piperidin-4-one

HRID 895126노트

반응식

HRID 895126 반응식
[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[N:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1.C(=O)([O-])[O-].[Na+].[Na+]>Cl.C(OCC)(=O)C.[Fe]>[NH2:8][C:6]1[CH:5]=[CH:4][C:3]([N:11]2[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]2)=[C:2]([F:1])[CH:7]=1

참가 물질

6

반응물 2

HCID 10340Sodium CarbonateHCID 37637811-(2-Fluoro-4-nitrophenyl)piperidin-4-one

생성물 1

HCID 223856071-(4-Amino-2-fluoro-phenyl)-piperidin-4-one

시약·촉매·용매 3

HCID 23925Iron촉매HCID 313Hydrochloric Acid용매HCID 8857Ethyl Acetate용매

실험 절차

Iron powder (16.4 g, 294 mmol) was slowly added to an ice-cold solution of 1-(2-fluoro-4-nitro-phenyl)-piperidin-4-one (7 g, 29.4 mmol), obtained in Preparation 5, in ethanolic HCl (50 ml) at 0° C. and stirred at the same temperature for 2 h. The reaction mixture was basified by the addition of sodium carbonate and pH of the solution was brought to 8. It was then diluted with ethyl acetate (100 ml) and the aqueous layer was separated. The aqueous layer was further extracted with ethyl acetate (100 ml×2). Combined organic extract was washed with water followed by brine and dried over sodium sulfate. Removal of volatiles left a pasty mass (7 g), which was used for the next step.

후처리

  1. customthe aqueous layer was separated
  2. extractionThe aqueous layer was further extracted with ethyl acetate (100 ml×2)
  3. extractionCombined organic extract
  4. washwas washed with water
  5. dry with materialdried over sodium sulfate
  6. customRemoval of volatiles
  7. waitleft a pasty mass (7 g), which

출처 및 근거

ORD 기록
ord-cfbf24ad9f084e0e857a029833035daf
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06914058B2

반응 노트

불러오는 중…