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Carbon Dioxide → N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide

HRID 1720416
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1720416
Cl.[CH3:2][NH2:3].[C:4](=[O:7])([O-])[O-].[K+].[K+].C(=O)=O.[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:16][C:15]=1[N:27]1[C:32](=[O:33])C2CCCC(=C2)C1=O.Cl>C(#N)C>[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:23][CH2:24][CH2:25][CH2:26]2)=[CH:16][C:15]=1[NH:27][C:32](=[O:33])[C:14]1[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=1[C:4]([NH:3][CH3:2])=[O:7]
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Komponenten

7

Edukt 5

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 6364545Methylamine hydrochlorideHCID 19425191N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimide

Produkt 1

HCID 19425267
N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide
Ausbeute 107,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Methylamine hydrochloride (0.200 g, 2.96 mmol) and potassium carbonate (0.400 g, 2.89 mmol), and acetonitrile (5 ml) as a solvent were placed into a round bottom flask (25 cc), followed by stirring at room temperature. After confirming the generation of carbon dioxide gas, N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimide (0.650 g, 1.79 mmol) was added thereto, followed by stirring overnight at room temperature. After completion of the reaction, the reaction mixture was poured into 1N hydrochloric acid (20 ml), and the mixture was extracted with ethyl acetate (40 ml x 3 portions). After drying the organic layer over anhydrous magnesium sulfate, the drying agent was removed, and the solvent was distilled off under reduced pressure. The precipitated crystals were isolated by filtration, thoroughly washed with hexane and dried to obtain N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide as white crystals (0.380 g, 53.8% yield). The melting point and the spectral data thereof are shown in Example 37.

Aufarbeitung

  1. additionwas added
  2. stirringby stirring overnight at room temperature
  3. customAfter completion of the reaction
  4. extractionthe mixture was extracted with ethyl acetate (40 ml x 3 portions)
  5. dry with materialAfter drying the organic layer over anhydrous magnesium sulfate
  6. customthe drying agent was removed
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe precipitated crystals were isolated by filtration
  9. washthoroughly washed with hexane
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-33a7cf0cbe024b3b826725e3f48c613b
Quelldatensatz
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05506190

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