Reaktionsgleichung
[CH3:1][C:2]([NH:6][CH3:7])([CH3:5])[CH2:3][OH:4].[CH2:8]1[O:18][C:17]2[CH:16]=[CH:15][C:12]([CH2:13]Cl)=[CH:11][C:10]=2[O:9]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:1][C:2]([N:6]([CH2:13][C:12]1[CH:15]=[CH:16][C:17]2[O:18][CH2:8][O:9][C:10]=2[CH:11]=1)[CH3:7])([CH3:5])[CH2:3][OH:4]Komponenten
Versuchsvorschrift
A mixture of 2-methyl-2-methylaminopropanol (1.5 g), 3,4-methylenedioxybenzyl chloride (2.5 g) and potassium carbonate (2 g) in acetonitrile (50 ml) was heated under reflux for 4 hours and evaporated. The residue was partitioned between ether and 2M hydrochloric acid and the acidic layer was washed with methylene chloride, basified with 10% aqueous sodium carbonate solution and extracted into methylene chloride. The organic extract was dried over magnesium sulphate and evaporated to give essentially pure 2-methyl-2-[N-(3,4-methylenedioxybenzyl)-N-methylamino]propanol as a yellow oil (2.0 g, 58%) which was used directly in Example 34. A small portion of this product was dissolved in ether and the solution was treated with excess saturated ethereal hydrogen chloride and evaporated. The residue was triturated with acetone/ethyl acetate to give the title compound as a colourless solid, m.p. 157°-159°.
Aufarbeitung
- temperaturewas heated
- temperatureunder reflux for 4 hours
- customevaporated
- customThe residue was partitioned between ether and 2M hydrochloric acid
- washthe acidic layer was washed with methylene chloride
- extractionextracted into methylene chloride
- extractionThe organic extract
- dry with materialwas dried over magnesium sulphate
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-918dbfc0cb474489870cd382c91a5f79
- Quelldatensatz
- uspto-grants-1993_03
- Patentnummer
- US05192765
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