Dimethylformamide → 1,3,3-Trimethylpiperazine-2,5-dione

HRID 1437249노트

반응식

HRID 1437249 반응식
N1CCCC[CH2:2]1.C(O[C:10](=O)[CH2:11][N:12]([C:14](=[O:16])C)C)C.[CH3:18][N:19]([CH3:22])[CH:20]=[O:21]>>[CH3:18][N:19]1[CH2:22][C:14](=[O:16])[NH:12][C:11]([CH3:10])([CH3:2])[C:20]1=[O:21]

참가 물질

4

반응물 3

HCID 6228Dimethylformamide2회HCID 8082PiperidineHCID 23090132Ethyl N-acetyl-N-methylglycinate

생성물 1

HCID 230901071,3,3-Trimethylpiperazine-2,5-dione수율 59%

실험 절차

Piperidine (867 mL) was added to N-[(α,α-dimethyl-(9H-fluoren-9-ylmethoxy)carbamino] acetylsarcosine ethyl ester (743 mg) in N,N-dimethylformamide (20 mL), followed by stirring at room temperature for 1 hour. N,N-Dimethylformamide (60 mL) was added thereto. The resultant mixture was stirred at 80° C. for 14 hours, and cooled in air. The reaction solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate, and then to the resultant solution, hexane was added. The precipitated crystals were recovered by filtration, to thereby give the title compound (162 mg, 59%).

후처리

  1. temperaturecooled in air
  2. customThe reaction solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. additionto the resultant solution, hexane was added
  5. filtrationThe precipitated crystals were recovered by filtration

출처 및 근거

ORD 기록
ord-34b15116a7234665bd6ee65e4339cd7a
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622471B2

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