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Ammonium formate → N,N-dimethylmorpholine-2-carboxamide

HRID 1914043
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HRID 1914043 반응식
C([N:8]1[CH2:13][CH2:12][O:11][CH:10]([C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[CH2:9]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CCO.[Pd]>[CH3:17][N:16]([CH3:18])[C:14]([CH:10]1[O:11][CH2:12][CH2:13][NH:8][CH2:9]1)=[O:15]
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참가 물질

5

반응물 2

HCID 2723923Ammonium formate2회HCID 711385114-benzyl-N,N-dimethylmorpholine-2-carboxamide

생성물 1

HCID 20472122N,N-dimethylmorpholine-2-carboxamide수율 99%

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 702Ethanol용매

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온도
50 °C

실험 절차

A mixture of 4-benzyl-N,N-dimethylmorpholine-2-carboxamide (803 mg, 3.23 mmol), ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) in EtOH (20 mL) was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated, and the residue was dissolved in EtOH (20 mL). Ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) were added to the mixture. The mixture was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated to afford desired product (506 mg, 98.9%) as colorless oil.

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationthe catalyst was filtered off
  3. washwashed with EtOH
  4. concentrationThe combined filtrate and washings were concentrated
  5. dissolutionthe residue was dissolved in EtOH (20 mL)
  6. temperatureThe mixture was heated at 50° C. for 1 hour
  7. temperatureAfter cooling to room temperature
  8. filtrationthe catalyst was filtered off
  9. washwashed with EtOH
  10. concentrationThe combined filtrate and washings were concentrated

출처 및 근거

ORD 기록
ord-25c055a7a16c471fb048b310c0e74a8d
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08609688B2

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