Ethanol → [2-(2-Aminoethyl)-4,5-dimethoxyphenyl]acetonitrile
Reaktionsgleichung
[C:1]([CH2:3][C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH3:13])=[CH:6][C:5]=1[CH2:14][CH2:15][NH:16]C(=O)C(F)(F)F)#[N:2].C(O)C.C(=O)([O-])[O-].[K+].[K+]>O>[NH2:2][CH2:1][CH2:3][C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH3:13])=[CH:6][C:5]=1[CH2:14][C:15]#[N:16]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Heat, at 50° C., a mixture of N-{2-[2-(cyanomethyl)-4,5-dimethoxyphenyl]ethyl}-2,2,2-trifluoroacetamide (20.5 g, 64.8 mmoles), ethanol (160 mL), potassium carbonate (13.2 g, 97.2 mmoles) and water (40 mL). After being in contact for 1 hour 30 minutes, extract the mixture by adding 200 mL of dichloromethane and 100 mL of saturated aqueous NaCl solution. Extract the aqueous phase with 100 mL of dichloromethane. Combine the organic phases, wash them with saturated aqueous NaCl solution (100 mL), dry them over MgSO4 and carry out drying in vacuo to obtain 10 g of a yellow oil corresponding to the title compound.
Aufarbeitung
- extractionextract the mixture
- additionby adding 200 mL of dichloromethane and 100 mL of saturated aqueous NaCl solution
- extractionExtract the aqueous phase with 100 mL of dichloromethane
- washwash them with saturated aqueous NaCl solution (100 mL)
- dry with materialdry them over MgSO4
- customcarry out drying in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-1d189e75c9634fadb2e94355772fedd2
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08835627B2
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