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Piperazine → HCID 66754327, 화합물

HRID 2167182
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HRID 2167182 반응식
FC1C(O[C:9]([CH:11]2[CH2:15][C:14](=[O:16])[NH:13][CH2:12]2)=[O:10])=C(F)C(F)=C(F)C=1F.[NH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(Cl)Cl>C1COCC1>[N:21]1([C:9]([CH:11]2[CH2:12][NH:13][C:14](=[O:16])[CH2:15]2)=[O:10])[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1
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참가 물질

5

반응물 3

HCID 4837PiperazineHCID 6344DichloromethaneHCID 866401555-Oxo-pyrrolidine-3-carboxylic acid pentafluorophenyl ester

생성물 1

HCID 66754327HCID 66754327, 화합물수율 107%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 5-oxo-pyrrolidine-3-carboxylic acid pentafluorophenyl ester 17 (40.1 mg, 0.0578 mmol) in 2 mL THF extra dry was added piperazine (19.9 mg, 0.231 mmol) at room temperature. The reaction mixture was stirred for 10 hours at room temperature. Afterwards, 20 mL methylene chloride were added. The resulting organic layer was washed with 20 mL of a saturated aqueous solution of sodium hydrogenocarbonate, dried over magnesium sulfate and the solvent was removed in vacuo. Finally, the crude product was purified by chromatography on silica gel (ethyl acetate:methanol 9:1→1:1) to afford the desired 4-(piperazine-1-carbonyl)-pyrrolidin-2-one 18 as a white solid (12.2 mg, 45.91%).

후처리

  1. customdry
  2. washThe resulting organic layer was washed with 20 mL of a saturated aqueous solution of sodium hydrogenocarbonate
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. customFinally, the crude product was purified by chromatography on silica gel (ethyl acetate:methanol 9:1→1:1)

출처 및 근거

ORD 기록
ord-f0bd907618e4449094423690572dd5ca
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09045414B2

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