Dichlorophen → 2,10-dichloro-12H-dibenzo[d,g][1,3]dioxocine
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:17])=[C:6]([CH2:8][C:9]2[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=2[OH:16])[CH:7]=1.I[CH2:19]I.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:17][CH2:19][O:16][C:10]3[CH:11]=[CH:12][C:13]([Cl:15])=[CH:14][C:9]=3[CH2:8][C:6]=2[CH:7]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 105 °C
Versuchsvorschrift
To a solution of bis-(5-chloro-2-hydroxyphenyl)-methane (24.4 g, 90.7 mmol) in dry DMF (340 mL) was added diiodomethane (25.5 g, 95.0 mmol) and potassium carbonate (18.2 g, 132 mmol). The mixture was stirred at 105° C. for 16 h. The mixture was added to ice water (1200 mL) and stirred for 30 min. The product was isolated by filtration, and washed with water and suspended in a mixture of ethanol (200 mL) and 4N NaOH (50 mL). The mixture was heated at 80° C. for 1 h. The mixture was added to water (600 mL) and 21.45 g (84%) 2,10-dichloro-12H-dibenzo[d,g][1,3]-dioxocin was isolated by filtration.
Aufarbeitung
- stirringstirred for 30 min
- customThe product was isolated by filtration
- washwashed with water
- additionsuspended in a mixture of ethanol (200 mL) and 4N NaOH (50 mL)
- temperatureThe mixture was heated at 80° C. for 1 h
- additionThe mixture was added to water (600 mL)
Quellen und Nachweise
- ORD-Eintrag
- ord-68571ba914494e319af7ee49a194dc8d
- Quelldatensatz
- uspto-grants-2004_04
- Patentnummer
- US06723731B2
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