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Water → Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate

HRID 1425296
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1425296
OC1CCC([C:8]2[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=2[C:10]([O:12][CH2:13][CH3:14])=[O:11])=CC1.CS(Cl)(=O)=O.[N-]=[N+]=[N-].[Na+].O.[C:29]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(O[C:56]([O:58][C:59]([CH3:62])([CH3:61])[CH3:60])=[O:57])(OC(C)(C)C)=O.[N:63]1[CH:68]=[CH:67][CH:66]=[CH:65][CH:64]=1>C(OCC)(=O)C>[C:59]([O:58][C:56]([NH:63][CH:68]1[CH2:67][CH2:66][C:65]([C:18]2[CH:8]=[C:9]([CH:15]=[CH:16][CH:17]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:64][CH2:29]1)=[O:57])([CH3:60])([CH3:61])[CH3:62]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 7

HCID 962WaterHCID 1049PyridineHCID 11776TriphenylphosphineHCID 31297Methanesulfonyl chlorideHCID 33557Sodium AzideHCID 90495Di-tert-butyl dicarbonateHCID 86648765HCID 86648765, Verbindung

Produkt 1

HCID 67548489Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of ethyl (4-hydroxycyclohex-1-enyl)benzoate obtained in Example (195a) (1 g, 4.06 mmol) in pyridine (20 mL) was cooled to 0° C. Methanesulfonyl chloride (628 μL, 8.12 mmol) was added at the same temperature, and the mixture was stirred at 0° C. for two hours. The reaction solution was diluted with ethyl acetate, washed with 1 N hydrochloric acid and brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was dissolved in N,N-dimethylformamide (30 mL). Sodium azide (1.32 g, 20.3 mmol) was added at room temperature, and the mixture was stirred at 70° C. for 18 hours. The reaction solution was diluted with ethyl acetate, washed with brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was dissolved in tetrahydrofuran (30 mL). Water (109 μL, 6.09 mmol) and triphenylphosphine (1.17 g, 4.47 mmol) were added at room temperature, and the mixture was stirred at room temperature for 18 hours. After 18 hours, di-tert-butyl dicarbonate (975 mg, 4.47 mmol) was added, and the mixture was stirred at room temperature for five hours. The reaction solution was diluted with ethyl acetate, washed with brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=2/1) to obtain 510 g of the title compound as a yellow oily substance (32%).

Aufarbeitung

  1. washwashed with 1 N hydrochloric acid and brine
  2. dry with materialdried over magnesium sulfate
  3. customThereafter, the solvent was evaporated under reduced pressure
  4. dissolutionThe resulting residue was dissolved in N,N-dimethylformamide (30 mL)
  5. stirringthe mixture was stirred at 70° C. for 18 hours
  6. washwashed with brine
  7. dry with materialdried over magnesium sulfate
  8. customThereafter, the solvent was evaporated under reduced pressure
  9. dissolutionThe resulting residue was dissolved in tetrahydrofuran (30 mL)
  10. stirringthe mixture was stirred at room temperature for 18 hours
  11. waitAfter 18 hours
  12. stirringthe mixture was stirred at room temperature for five hours
  13. washwashed with brine
  14. dry with materialdried over magnesium sulfate
  15. customThereafter, the solvent was evaporated under reduced pressure
  16. customThe resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=2/1)

Quellen und Nachweise

ORD-Eintrag
ord-a70e16776c194090acf6d6b92aef5180
Quelldatensatz
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08927588B2

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