HCID 20406152, Verbindung → Methanone, (2-amino-5-methylphenyl)(4-fluorophenyl)-
Reaktionsgleichung
[F:1][C:2]1[CH:20]=[CH:19][C:5]([C:6]([C:8]2[CH:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:9]=2[NH:15]C(=O)C)=[O:7])=[CH:4][CH:3]=1>C(O)C.Cl>[NH2:15][C:9]1[CH:10]=[CH:11][C:12]([CH3:14])=[CH:13][C:8]=1[C:6]([C:5]1[CH:19]=[CH:20][C:2]([F:1])=[CH:3][CH:4]=1)=[O:7]Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A solution of 119 g (0.44 mole of N-[2-(4-fluorobenzoyl)-4-methylphenyl]acetamide in 500 ml of 95% ethanol and 300 ml of 6N hydrochloric acid was heated at reflux for 16 hr. The solvents were removed on a roto-evaporator and the residue obtained was partitioned between concentrated ammonium hydroxide and benzene. The organic layer was concentrated and the new residue was chromatographed on silica gel, eluting with 10% ethyl acetate in hexane. The product fractions were concentrated and the residue was crystallized from a mixture of cyclohexane and hexane to give 56.3 g (61.5%) of the titled compound as bright yellow crystals, m.p. 70.0°-71.5° C.
Aufarbeitung
- temperatureat reflux for 16 hr
- customThe solvents were removed on a roto-evaporator
- customthe residue obtained
- customwas partitioned between concentrated ammonium hydroxide and benzene
- concentrationThe organic layer was concentrated
- customthe new residue was chromatographed on silica gel
- washeluting with 10% ethyl acetate in hexane
- concentrationThe product fractions were concentrated
- customthe residue was crystallized from a mixture of cyclohexane and hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-ce1a0d64d9574e01bf7a2c3c022d8ff6
- Quelldatensatz
- uspto-grants-1985_03
- Patentnummer
- US04503073
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