Reaktionsgleichung
[CH3:1][CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[CH2:3][CH3:4].Cl[CH2:14][CH2:15][NH:16][C:17](=[O:20])[O:18][CH3:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:1][CH:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:14][CH2:15][NH:16][C:17](=[O:20])[O:18][CH3:19])=[CH:10][CH:11]=1)[CH2:3][CH3:4]Komponenten
6
Versuchsvorschrift
A mixture of 4-(1-methylpropoxy)phenol (9.2 mmol), methyl 2-chloroethylcarbamate (11.9 mmol), and potassium carbonate (18.4 mmol) in 20 ml of dimethylformamide (DMF) is heated at 85° for 18 hours. The reaction mixture is cooled to room temperature (RT), poured into water and extracted with ether. The combined ether extracts are washed with water until neutral, followed with brine and dried over calcium sulfate. The solvent is removed in vacuo and the residue is placed under high vacuum at 80° for ca. 2 hours to remove the excess methyl 2-chloroethylcarbamate. Purification by preparative thin layer chromatography (prep. TLC) gives methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate.
Aufarbeitung
- temperatureis heated at 85° for 18 hours
- extractionextracted with ether
- washThe combined ether extracts are washed with water until neutral,
- dry with materialdried over calcium sulfate
- customThe solvent is removed in vacuo
- customto remove the excess methyl 2-chloroethylcarbamate
- customPurification by preparative thin layer chromatography (prep. TLC)
Quellen und Nachweise
- ORD-Eintrag
- ord-add4aaf646714895ab7b855a5ef88067
- Quelldatensatz
- uspto-grants-1987_09
- Patentnummer
- US04697033
Verknüpfte Notizen
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