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Ammonium formate → 2-(Pyrrolidin-3-yl)pyridine

HRID 1742845
ノート
印刷プレビュー

反応式

HRID 1742845 の反応式
C1(C[N:8]2[CH2:12][CH2:11][CH:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)[CH2:9]2)C=CC=CC=1.C([O-])=O.[NH4+]>[Pd].CO.O>[NH:8]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)[CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 2723923Ammonium formateHCID 109556222-(1-Benzylpyrrolidin-3-yl)pyridine

生成物 1

HCID 50139382-(Pyrrolidin-3-yl)pyridine収率 75%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a suspension of 2-[1-(phenylmethyl)-3-pyrrolidinyl]pyridine (7.15 g, 30.0 mmol) and 10% palladium on charcoal catalyst (1.90 g) in methanol (120 mL) was added dropwise a solution of ammonium formate (7.57 g, 120 mmol) in water (30 mL). The mixture was heated at reflux for 30 minutes, allowed to cool to room temperature, and filtered. The filtrate was concentrated under reduced pressure, the residue was taken up in water (10 mL), and the solution was made basic with concentrated ammonia and extracted with dichloromethane (4×15 mL). The organic extracts were combined, dried over anhydrous potassium carbonate, and concentrated to a yellow oil. This crude product was chromatographed (silica gel, chloroform-methanol-ammonia 75:25:5) to give the title compound (3.33 g, 75%) as a faint yellow liquid.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. extractionextracted with dichloromethane (4×15 mL)
  6. dry with materialdried over anhydrous potassium carbonate
  7. concentrationconcentrated to a yellow oil
  8. customThis crude product was chromatographed (silica gel, chloroform-methanol-ammonia 75:25:5)

出典と根拠

ORDレコード
ord-bf693ce45a1840188320f3601baa7a65
出典データセット
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05342844

反応ノート

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