Sodium borohydride → 2,2-diethoxy-N-(thiophen-2-ylmethyl)ethanamine
Reaktionsgleichung
[CH2:1]([O:3][CH:4]([O:13][CH2:14][CH3:15])[CH2:5][N:6]=[CH:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)[CH3:2].[BH4-].[Na+]>C(O)C>[CH2:14]([O:13][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][NH:6][CH2:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)[CH3:15]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2,2-Diethoxy-N-(thiophen-2-ylmethylene)ethaneamine (100 g) prepared in the step 1 was dissolved in 500 mL of dry ethanol, then 18.3 g of sodium borohydride was slowly added thereto little by little at room temperature and the mixture was stirred overnight at room temperature. The solvent was evaporated from the reaction solution in vacuo and the residue was poured over 300 mL of a 10% aqueous solution of acetic acid. The resulting aqueous solution was washed with diethyl ether, neutralized with 10% aqueous ammonia and subjected to extraction with diethyl ether. The organic layer was washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo to give 72.5 g of the objective compound as colorless liquid.
Aufarbeitung
- customThe solvent was evaporated from the reaction solution in vacuo
- additionthe residue was poured over 300 mL of a 10% aqueous solution of acetic acid
- washThe resulting aqueous solution was washed with diethyl ether
- extractionsubjected to extraction with diethyl ether
- washThe organic layer was washed with water
- dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
- customthe solvent was evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-d5921d32063e4ba0b245f82bc0d86b5c
- Quelldatensatz
- uspto-grants-2012_07
- Patentnummer
- US08217031B2
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