Hydrochloric Acid → 4-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

HRID 7883

Reaktionsgleichung

Reaktionsgleichung von HRID 7883
[CH2:1]([C:5]12[CH2:17][CH2:16][C:15](=[O:18])[C:14]([C:19]([O:21]CC)=[CH2:20])=[C:13]1[C:12]1[C:7](=[C:8]([Cl:26])[C:9]([O:24][CH3:25])=[CH:10][CH:11]=1)[CH2:6]2)[CH2:2][CH2:3][CH3:4].Cl>C(O)C.O>[C:19]([C:14]1[C:15](=[O:18])[CH2:16][CH2:17][C:5]2([CH2:1][CH2:2][CH2:3][CH3:4])[C:13]=1[C:12]1[C:7](=[C:8]([Cl:26])[C:9]([O:24][CH3:25])=[CH:10][CH:11]=1)[CH2:6]2)(=[O:21])[CH3:20]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 219909099a-butyl-8-chloro-4-(1-ethoxyvinyl)-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

Produkt 1

HCID 219908794-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

The product from step 1 in ethanol (1.0 mL), water (0.2 mL) and aqueous 2N HCl (0.2 mL) was stirred and heated in an oil bath at 80° C. for 40 minutes. After cooling, the mixture was partitioned between EtOAc (20 mL) and water (20 mL). The organic phase was washed with brine (20 mL), dried over MgSO4, filtered, and evaporated under vacuum to provide 4-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (54 mg) as an oil.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe mixture was partitioned between EtOAc (20 mL) and water (20 mL)
  3. washThe organic phase was washed with brine (20 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-194006f950674b50a93e6edc19549752
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07087599B2

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