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

HRID 546615

反応式

HRID 546615 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 5778004-(Pyrrolidin-1-ylcarbonyl)aniline収率 115.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-976bb117e69147dfb22da00f6c7266ef
出典データセット
uspto-grants-2011_05
特許番号
US07935819B2

関連ノート

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