Lithium Hydroxide → 1-(4-Chlorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one

HRID 458143Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 458143
FC(F)(F)C1C=C(C=C(C(F)(F)F)C=1)C([N:8]1[CH2:25][CH2:24][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)[CH2:14][NH:13][C:12]2=[O:23])[CH2:10][CH2:9]1)=O.[Li+].[OH-]>C1COCC1.O.CO>[Cl:22][C:19]1[CH:20]=[CH:21][C:16]([N:15]2[C:11]3([CH2:10][CH2:9][NH:8][CH2:25][CH2:24]3)[C:12](=[O:23])[NH:13][CH2:14]2)=[CH:17][CH:18]=1

Komponenten

6

Edukt 2

HCID 3939Lithium HydroxideHCID 18401639HCID 18401639, Verbindung

Produkt 1

HCID 201607621-(4-Chlorophenyl)-1,3,8-triazaspiro[4.5]decan-4-oneAusbeute 69,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a mixture of 1.5 g (2.97 mmol) 8-(3,5-bis-trifluoromethyl-benzoyl)-1-(4-chloro-phenyl)-1,3,8-triaza-spiro[4.5]decan-4-one in 4.5 ml THF, 4.5 ml water and 4.5 ml methanol were added 0.85 g (35.6 mmol) powdered LiOH. The reaction mixture was stirred at ambient temperature for 48 hours. The solvent was removed in vacuo. The residue was stirred in water. The resulting solid was filtered, washed with water and dried to provide the title compound (0.55 g) as a colorless solid; MS (ISP): 266.1 MH+.

Aufarbeitung

  1. additionwere added 0.85 g (35.6 mmol)
  2. customThe solvent was removed in vacuo
  3. stirringThe residue was stirred in water
  4. filtrationThe resulting solid was filtered
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d82fdf1bee7d4126860f1c4ed2b664a9
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07189850B2

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