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Ethanol → N-(3-Fluoro-4-methyl-5,6,7,8-tetrahydro-1-naphthyl)acetamide

HRID 355979
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 355979
[F:1][C:2]1[C:11]([CH3:12])=[C:10]2[C:5]([CH2:6][CH2:7][CH2:8][C:9]2=O)=[C:4]([N+:14]([O-])=O)[CH:3]=1.[CH2:17]([OH:19])[CH3:18].[BH4-].[Na+]>C1COCC1>[C:17]([NH:14][C:4]1[CH:3]=[C:2]([F:1])[C:11]([CH3:12])=[C:10]2[C:5]=1[CH2:6][CH2:7][CH2:8][CH2:9]2)(=[O:19])[CH3:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 702EthanolHCID 4311764Sodium borohydrideHCID 224494067-Fluoro-8-methyl-5-nitro-3,4-dihydronaphthalen-1(2H)-one

Produkt 1

HCID 10799012N-(3-Fluoro-4-methyl-5,6,7,8-tetrahydro-1-naphthyl)acetamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

The compound obtained in (4) above (1.35 gm) was dissolved into 5 ml of ethanol and 15 ml of THF. To the solution was added 114 mg of sodium borohydride while stirring at room temperature. After stirring for 20 minutes, the reaction mixture was concentrated. To the concentrate were added 25 ml of toluene and 840 mg of p-TsOH, followed by heating under reflux for 30 minutes. Upon the addition of 100 ml of ethyl acetate, the reaction product was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was dissolved into 20 ml of ethyl acetate and catalytically hydrogenated with the addition of 400 mg of platinum oxide for 4 hours. The catalyst was removed, the filtrate was concentrated, and 10 ml of dichloromethane was added to the concentrate. After the further addition of 1.2 ml of triethylamine and 0.81 ml of acetic anhydride, the mixture was stirred for 40 minutes. The reaction product was diluted with 50 ml of chloroform, washed with dilute hydrochloric acid, saturated sodium bicarbonate and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated to obtain 1.23 gm of the title compound.

Aufarbeitung

  1. stirringAfter stirring for 20 minutes
  2. concentrationthe reaction mixture was concentrated
  3. additionTo the concentrate were added 25 ml of toluene and 840 mg of p-TsOH
  4. temperatureby heating
  5. temperatureunder reflux for 30 minutes
  6. additionUpon the addition of 100 ml of ethyl acetate
  7. washthe reaction product was washed with saturated brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe solvent was evaporated
  10. dissolutionthe residue was dissolved into 20 ml of ethyl acetate and catalytically hydrogenated with the addition of 400 mg of platinum oxide for 4 hours
  11. customThe catalyst was removed
  12. concentrationthe filtrate was concentrated
  13. addition10 ml of dichloromethane was added to the concentrate
  14. additionAfter the further addition of 1.2 ml of triethylamine and 0.81 ml of acetic anhydride
  15. stirringthe mixture was stirred for 40 minutes
  16. additionThe reaction product was diluted with 50 ml of chloroform
  17. washwashed with dilute hydrochloric acid, saturated sodium bicarbonate and saturated brine in this order
  18. dry with materialdried over anhydrous sodium sulfate
  19. customThe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-41d48cefadde48fca38478b602ebe194
Quelldatensatz
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05834476

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