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Boron Trichloride → (3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one

HRID 898215
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 898215
[CH2:1]([C@H:3]1[N:12]([C:13](=[O:22])[C:14]2[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([F:23])=[CH:9][CH:10]=2)[N:5]([CH3:24])[C:4]1=[O:25])[CH3:2].B(Cl)(Cl)Cl>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(Cl)Cl>[CH2:1]([C@H:3]1[N:12]([C:13](=[O:22])[C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([F:23])=[CH:9][CH:10]=2)[N:5]([CH3:24])[C:4]1=[O:25])[CH3:2]
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Komponenten

5

Edukt 2

HCID 25135Boron TrichlorideHCID 69223654(3R)-3-ethyl-7-fluoro-4-(4-methoxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one

Produkt 1

HCID 11709655(3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-oneAusbeute 88,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 67553Tetrabutylammonium IodideKatalysator
HCID 6344
Dichloromethane
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a stirred solution of (3R)-3-ethyl-7-fluoro-4-(4-methoxybenzoyl)-1-methyl-3,4 dihydroquinoxalin-2(1H)-one (0.19 g, 0.55 mmol) and tetrabutylammonium iodide (0.41 g, 1.1 mmol) in methylene chloride (5 mL), under nitrogen, at −78° C., was added a 1.0 M solution of boron trichloride in methylene chloride (2.8 mL, 2.8 mmol). Stirring was continued at −78° C. for 5 minutes, and the reaction was warmed to 0° C. where it was stirred for 5 h. The reaction was quenched by the addition of ice water, and the resulting mixture was stirred for 10 min. The layers were separated. The organic layer was washed with water and brine and dried over magnesium sulfate. Evaporation of the solvent and purification by eluting it through a short plug of silica gel with 75% hexane/EtOAc gave 0.16 g (88%) of (3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one. [α]D25=−300° (c=0.009 G/ML, DMSO); MS (ESI) m/z 329 ([M+H]+); MS (ESI) m/z 327 ([M−H]−); HRMS: calcd for C18H17FN2O3, 328.1223; found (ESI+), 329.13036; Anal. Calcd for C18H17FN2O3: C, 65.85; H, 5.22; N, 8.53. Found: C, 65.73; H, 5.46; N, 8.28.

Aufarbeitung

  1. stirringwas stirred for 5 h
  2. customThe reaction was quenched by the addition of ice water
  3. stirringthe resulting mixture was stirred for 10 min
  4. customThe layers were separated
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customEvaporation of the solvent and purification
  8. washby eluting it through a short plug of silica gel with 75% hexane/EtOAc

Quellen und Nachweise

ORD-Eintrag
ord-823f9168a24346eb86dfbb95ef91d0f9
Quelldatensatz
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07351709B2

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