Reaktionsgleichung
S(Cl)(Cl)=O.[CH3:5][O:6][C:7]1[C:14]([O:15][CH3:16])=[CH:13][CH:12]=[CH:11][C:8]=1CO.N1C(C)=CC=CC=1C.[CH2:25](Cl)[Cl:26]>>[CH3:16][O:15][C:14]1[CH:13]=[C:12]([CH:11]=[CH:8][C:7]=1[O:6][CH3:5])[CH2:25][Cl:26]Komponenten
5
Versuchsvorschrift
Thionyl chloride (288 g) is added over 1.5 hour to a stirred solution of 2,3-dimethoxybenzyl alcohol (400 g) and 2,6-lutidine in methylene chloride (2 l). The reaction mixture is then stirred for 30 minutes after which it is washed with 2 N hydrochloric acid (7×1 l) and then with water. The organic layer is separated, dried (MgSO4) and evaporated to give a residue, which upon distillation yields 3,4-dimethoxybenzyl chloride (375 g), b.p. 145°-150° C. at 20-25 nm (waterpump vacuum). The material solidifies on standing.
Aufarbeitung
- washis washed with 2 N hydrochloric acid (7×1 l)
- customThe organic layer is separated
- dry with materialdried (MgSO4)
- customevaporated
- customto give a residue, which
- distillationupon distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-1440990bfe9342988351331b381fd1f2
- Quelldatensatz
- uspto-grants-1982_08
- Patentnummer
- US04342780
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