N-(1-benzylpiperidin-4-yl)-2,2,2-trifluoroacetamide → 2,2,2-trifluoro-N-(piperidin-4-yl)acetamide

HRID 1634060ノート

反応式

HRID 1634060 の反応式
C([O-])=O.[NH4+].[F:5][C:6]([F:24])([F:23])[C:7]([NH:9][CH:10]1[CH2:15][CH2:14][N:13](CC2C=CC=CC=2)[CH2:12][CH2:11]1)=[O:8]>[Pd].CO>[F:24][C:6]([F:5])([F:23])[C:7]([NH:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[O:8]

参加物

5

反応物 2

HCID 1531300N-(1-benzylpiperidin-4-yl)-2,2,2-trifluoroacetamideHCID 2723923Ammonium formate

生成物 1

HCID 107742532,2,2-trifluoro-N-(piperidin-4-yl)acetamide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒2 回

反応条件

温度
5 °C

実験手順

A 500 mL, three-necked round-bottomed flask under nitrogen was charged with 4 g of 10% Palladium on Carbon, and 100 mL of methanol. The suspension was cooled to 5° C. and 10 g of ammonium formate was added in one batch (evolution of gas was observed). A solution of 10 g (35 mmol) of the 4-trifluoroacetamido-1-benzylpiperidine in 100 mL of methanol was then added dropwise gradually. The resulting reaction mixture was refluxed for 2.5 hr. and then at room temperature overnight. The catalyst was filtered off through Celite under a blanket of nitrogen and washed with ethanol. The filtrate was concentrated under reduced pressure to give 6.9 g (quantitative yield) of a light yellow solid of the title compound.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 2.5 hr
  3. customat room temperature
  4. customovernight
  5. filtrationThe catalyst was filtered off through Celite under a blanket of nitrogen
  6. washwashed with ethanol
  7. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-dfd2ecebe6804fa5b1cb67b841bed5d8
出典データセット
uspto-grants-2003_01
特許番号
US06506749B2

反応ノート

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