Hexamethylenetetramine → 4-(2',6'-Dichlorobenzyl)oxazole
Reaktionsgleichung
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:3]=1[CH2:4][C:5]([CH:7]=[O:8])=O.[CH2:14]1N2CN3CN(C2)C[N:15]1C3.C([O-])(=O)C.[NH4+]>C(N)=O>[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:3]=1[CH2:4][C:5]1[N:15]=[CH:14][O:8][CH:7]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
21.7 g of crude 2,6-dichlorobenzylglyoxal are dissolved in 50 ml of formamide. 7.0 g of hexamethylenetetramine and 30.8 g of ammonium acetate are added and the reaction mixture is stirred at 100° C. for 2 hours, then is evaporated to dryness in vacuo. 200 ml of water are added and the pH of the aqueous phase is adjusted, while stirring, to 2-3 with concentrate hydrochloric acid. The solution is washed with toluene (3×50 ml). The aqueous solution is made alkaline with sodium hydroxide (pH=8-9) and then extracted three times with chloroform (1×100 ml and 2×50 ml). The combined chloroform extracts are washed with water, dried with sodium sulfate and evaporated to dryness. The residue, which consisted of crude product, is used in step (c) below.
Aufarbeitung
- customis evaporated to dryness in vacuo
- addition200 ml of water are added
- stirringwhile stirring, to 2-3 with concentrate hydrochloric acid
- washThe solution is washed with toluene (3×50 ml)
- extractionextracted three times with chloroform (1×100 ml and 2×50 ml)
- washThe combined chloroform extracts are washed with water
- dry with materialdried with sodium sulfate
- customevaporated to dryness
Quellen und Nachweise
- ORD-Eintrag
- ord-beaca45448a7416f9b2081a7557a3197
- Quelldatensatz
- uspto-grants-1984_04
- Patentnummer
- US04443466
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