1-Acetyl-3-[[3-methoxy-4-(trifluoromethyl)phenyl]methylene]piperazine-2,5-dione → 3-[3-Methoxy-4-(trifluoromethyl)benzyl]piperazine-2,5-dione

HRID 1375020노트

반응식

HRID 1375020 반응식
C([N:4]1[CH2:9][C:8](=[O:10])[NH:7][C:6](=[CH:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[C:14]([O:22][CH3:23])[CH:13]=2)[C:5]1=[O:24])(=O)C>O1CCCC1.[C].[Pd]>[CH3:23][O:22][C:14]1[CH:13]=[C:12]([CH:17]=[CH:16][C:15]=1[C:18]([F:21])([F:20])[F:19])[CH2:11][CH:6]1[NH:7][C:8](=[O:10])[CH2:9][NH:4][C:5]1=[O:24]

참가 물질

4

반응물 1

HCID 694200991-Acetyl-3-[[3-methoxy-4-(trifluoromethyl)phenyl]methylene]piperazine-2,5-dione

생성물 1

HCID 179642273-[3-Methoxy-4-(trifluoromethyl)benzyl]piperazine-2,5-dione수율 81.2%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 1-acetyl-3-[[3-methoxy-4-(trifluoromethyl)phenyl]methylene]piperazine-2,5-dione (1.8 g) in tetrahydrofuran (50 ml) was hydrogenated over 10% palladium-carbon (50% wet, 180 mg) for 5 hours at atmospheric pressure. After removal of the catalyst by filtration, the filtrate was added hydrazine monohydrate (395 mg). The mixture was stirred for 1.5 hours at room temperature and concentrated under reduced pressure. The residue was triturated with isopropyl ether (12 ml) and the precipitates were collected by filtration, and washed with isopropyl ether to give 3-[3-methoxy-4-(trifluoromethyl)benzyl]piperazine-2,5-dione (1.29 g) as a powder.

후처리

  1. customAfter removal of the catalyst
  2. filtrationby filtration
  3. additionthe filtrate was added hydrazine monohydrate (395 mg)
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was triturated with isopropyl ether (12 ml)
  6. filtrationthe precipitates were collected by filtration
  7. washwashed with isopropyl ether

출처 및 근거

ORD 기록
ord-c44734d33fe84fa8bf2463391e174e10
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07166598B2

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