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Water → ethyl (6-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate

HRID 1792931
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1792931
[H-].[Na+].[F:3][C:4]([F:21])([F:20])[C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[N:9]([CH2:15][CH:16]([CH3:18])[CH3:17])[CH:8]2O.[F:22][C:23]([F:40])([F:39])[C:24]1[CH:32]=[C:31]2[C:27]([CH:28](O)[N:29]([CH2:34][CH:35]([CH3:37])[CH3:36])[C:30]2=[O:33])=[CH:26][CH:25]=1.O.C[O:43][CH2:44][CH2:45]OC>>[F:3][C:4]([F:21])([F:20])[C:5]1[CH:6]=[C:7]2[C:11]([C:10](=[O:14])[N:9]([CH2:15][CH:16]([CH3:18])[CH3:17])[CH:8]2[CH2:45][C:44]([O:33][CH2:30][CH3:31])=[O:43])=[CH:12][CH:13]=1.[F:22][C:23]([F:40])([F:39])[C:24]1[CH:32]=[C:31]2[C:27](=[CH:26][CH:25]=1)[CH:28]([CH2:45][C:44]([O:14][CH2:10][CH3:11])=[O:43])[N:29]([CH2:34][CH:35]([CH3:37])[CH3:36])[C:30]2=[O:33]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 962WaterHCID 80711,2-DimethoxyethaneHCID 24758Sodium hydrideHCID 22025449HCID 22025449, VerbindungHCID 22025460HCID 22025460, Verbindung

Produkt 2

HCID 86591365ethyl (6-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate
HCID 86591366
ethyl (5-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

Ethyl (5-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate and ethyl (6-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate are prepared as described in Example 2, starting with 1.32 g of 60% sodium hydride in 120 cm3 of 1,2-dimethoxyethane, 6.57 cm3 of triethyl phosphonoacetate and 12.07 g of 5-trifluoromethyl-3-hydroxy-2-isobutyl-2,3-dihydroisoindol-1-one and 6-trifluoromethyl-3-hydroxy-2-isobutyl-2,3-dihydroisoindol-1-one. The mixture is refluxed for 24 hours and then cooled to a temperature in the region of 20° C. The reaction mixture is then treated with 150 cm3 of water and the mixture is then extracted with 3 times 250 cm3 of diethyl ether. The organic extracts are combined, washed with 150 cm3 of saturated brine, dried over magnesium sulfate, filtered and then concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. A mixture of 2.3 g of the residue is injected onto a column 8 cm in diameter containing 1.2 kg of Whelk OI,SS chiral stationary phase. The elution is performed with a mobile phase composed of a mixture of dichloromethane, ethanol and heptane in proportions of 14.5/0.5/85 v/v. Two additional injections of 2.7 g and 3 g are made under identical conditions. The fractions comprising the first regioisomer are combined and concentrated to dryness under reduced pressure (1 kPa) at a temperature in the region of 40° C. 1.86 g of ethyl (5-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate are thus obtained in the form of a white solid (Rf=0.64, thin layer chromatography on silica gel, eluent: cyclohexane/ethyl acetate (50/50 by volume)). The fractions comprising the second regioisomer are combined and concentrated to dryness under reduced pressure (1 kPa) at a temperature in the region of 40° C. to give 2.79 g of a white solid. This product is repurified by chromatography under argon pressure (80 kPa) on a cartridge of silica gel (particle size 32-63 μm), eluting with a mixture of cyclohexane/ethyl acetate (90/10 by volume). The fractions comprising the expected product are combined and concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. 1.25 g of ethyl (6-trifluoromethyl-2-isobutyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate are thus obtained in the form of a colorless viscous oil. (Rf=0.46, thin layer chromatography on silica gel, eluent: cyclohexane/ethyl acetate (75/25 by volume)).

Aufarbeitung

  1. temperatureThe mixture is refluxed for 24 hours
  2. extractionthe mixture is then extracted with 3 times 250 cm3 of diethyl ether
  3. washwashed with 150 cm3 of saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C
  7. additionA mixture of 2.3 g of the residue
  8. additioncontaining 1.2 kg of Whelk OI,SS chiral stationary phase
  9. washThe elution
  10. additioncomposed of a mixture of dichloromethane, ethanol and heptane in proportions of 14.5/0.5/85 v/v
  11. concentrationconcentrated to dryness under reduced pressure (1 kPa) at a temperature in the region of 40° C

Quellen und Nachweise

ORD-Eintrag
ord-b911b6e30eac40c5be3c86438d8fe792
Quelldatensatz
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07078428B2

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