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

HRID 1634060

반응식

HRID 1634060 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매2회

반응 조건

온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dfd2ecebe6804fa5b1cb67b841bed5d8
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06506749B2

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