Methanesulfonic Acid → 1,2-Dimethoxy-4-(2-methylphenylsulphonyl)-5-methylbenzene
Reaktionsgleichung
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.CS(O)(=O)=O.[CH3:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:23]=1[O:29][CH3:30].[CH3:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[S:38](O)(=[O:40])=[O:39]>>[CH3:30][O:29][C:23]1[CH:24]=[C:25]([CH3:28])[C:26]([S:38]([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=2[CH3:31])(=[O:40])=[O:39])=[CH:27][C:22]=1[O:21][CH3:20]Komponenten
Versuchsvorschrift
50 g of phosphorus pentoxide are covered, by pouring, with 400 ml of methanesulphonic acid and the whole is stirred at 60° until a clear solution has formed. 30.4 g (0.2 mol) of 1,2-dimethoxy-4-methylbenzene and 43 g (0.2 mol) of 2-methylbenzenesulphonic acid (80% strength) are then added, and the internal temperature is increased to 80° for 30 minutes. The mixture is poured onto 4 liters of ice-water and extracted with ethyl acetate. The extract solution is washed twice with water, dried over sodium sulphate, filtered and concentrated by evaporation in a rotary evaporator. The oil remaining crystallises immediately. It is triturated with diethyl ether and filtered off. In this manner colourless crystals of 1,2-dimethoxy-4-(2-methylphenylsulphonyl)-5-methylbenzene having a melting point of 126°-128° are obtained.
Aufarbeitung
- customhas formed
- temperaturethe internal temperature is increased to 80° for 30 minutes
- extractionextracted with ethyl acetate
- washThe extract solution is washed twice with water
- dry with materialdried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated by evaporation in a rotary evaporator
- customThe oil remaining crystallises immediately
- customIt is triturated with diethyl ether
- filtrationfiltered off
Quellen und Nachweise
- ORD-Eintrag
- ord-185eac5d815741e5845b015b06bc3790
- Quelldatensatz
- uspto-grants-1986_07
- Patentnummer
- US04600709
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