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Diethyl (ethoxymethylene)malonate → Ethyl 2-[(4-fluorophenyl)methyl]-8-hydroxy-1-oxo-3,4-dihydropyrrolo[1,2-a]pyrazine-7-carboxylate

HRID 494082
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인쇄 미리보기

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HRID 494082 반응식
[F:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][NH:10][CH2:9][C:8]2=[O:13])=[CH:4][CH:3]=1.C([O:18][CH:19]=[C:20]([C:26](OCC)=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22])C.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].C1COCC1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][N:10]3[CH:26]=[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:19]([OH:18])=[C:9]3[C:8]2=[O:13])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6871Diethyl (ethoxymethylene)malonateHCID 8028TetrahydrofuranHCID 2733832Lithium HexamethyldisilazideHCID 185386381-(4-Fluorobenzyl)piperazin-2-one

생성물 1

HCID 3011068Ethyl 2-[(4-fluorophenyl)methyl]-8-hydroxy-1-oxo-3,4-dihydropyrrolo[1,2-a]pyrazine-7-carboxylate

시약·촉매·용매 1

HCID 1140
Toluene
용매

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온도
80 °C

실험 절차

A mixture of 1-(4-fluorobenzyl)piperazin-2-one (10.0 g, 48.0 mmol) and diethyl ethoxymethylenemalonate (10.9 g, 50.4 mmol) in toluene (250 mL) was heated in a sealed tube at 80° C. for 4 hours. The resultant mixture was concentrated under vacuum. The residue was dissolved in anhydrous DMF (350 mL), cooled to 0° C. under an atmosphere of nitrogen, and treated with a solution of lithium bis(trimethylsilyl)amide in THF (1 M, 57.4 mL, 57.4 mmol). The reaction mixture was stirred at room temperature overnight and concentrated under vacuum. The residue was partitioned between ethyl acetate and dilute aqueous HCl. The organic extract was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated with diethyl ether, and the solid precipitated was filtered to provide the titled compound.

후처리

  1. concentrationThe resultant mixture was concentrated under vacuum
  2. dissolutionThe residue was dissolved in anhydrous DMF (350 mL)
  3. temperaturecooled to 0° C. under an atmosphere of nitrogen
  4. concentrationconcentrated under vacuum
  5. customThe residue was partitioned between ethyl acetate and dilute aqueous HCl
  6. extractionThe organic extract
  7. washwas washed with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under vacuum
  11. customThe residue was triturated with diethyl ether
  12. customthe solid precipitated
  13. filtrationwas filtered

출처 및 근거

ORD 기록
ord-fa1ec7bbb4644767a1f2ba9198566c11
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538112B2

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