(4-Nitrophenyl)(pyrrolidin-1-yl)methanone → 4-(Pyrrolidin-1-ylcarbonyl)aniline

HRID 546615노트

반응식

HRID 546615 반응식
[N+:1]([C:4]1[CH:16]=[CH:15][C:7]([C:8]([N:10]2[CH2:14][CH2:13][CH2:12][CH2:11]2)=[O:9])=[CH:6][CH:5]=1)([O-])=O.C([O-])=O.[NH4+]>CO.[Pd]>[N:10]1([C:8]([C:7]2[CH:15]=[CH:16][C:4]([NH2:1])=[CH:5][CH:6]=2)=[O:9])[CH2:11][CH2:12][CH2:13][CH2:14]1

참가 물질

5

반응물 2

HCID 386112(4-Nitrophenyl)(pyrrolidin-1-yl)methanoneHCID 2723923Ammonium formate

생성물 1

HCID 5778004-(Pyrrolidin-1-ylcarbonyl)aniline수율 115.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 1.28 g of 1-(4-nitrobenzoyl)pyrrolidine obtained in stage a) below in 50 mL of methanol are added, under argon, 4.26 g of ammonium formate and 9 mg of 10% palladium-on-charcoal. The reaction mixture is stirred at room temperature for 5 hours and then filtered through Celite and concentrated under reduced pressure. The residue is taken up in water and extracted with ethyl acetate. The organic phase is then washed with saturated sodium chloride solution, dried over magnesium sulphate, filtered and concentrated under reduced pressure to give 1.28 g of 4-(pyrrolidin-1-ylcarbonyl)aniline, the characteristics of which are as follows:

후처리

  1. filtrationfiltered through Celite
  2. concentrationconcentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is then washed with saturated sodium chloride solution
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-976bb117e69147dfb22da00f6c7266ef
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935819B2

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