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

HRID 1437249ノート

反応式

HRID 1437249 の反応式
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]

参加物

4

反応物 3

HCID 6228Dimethylformamide2 回HCID 8082PiperidineHCID 23090132Ethyl N-acetyl-N-methylglycinate

生成物 1

HCID 230901071,3,3-Trimethylpiperazine-2,5-dione収率 59%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-34b15116a7234665bd6ee65e4339cd7a
出典データセット
uspto-grants-2009_11
特許番号
US07622471B2

反応ノート

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