2-(Methylamino)ethanol → HCID 68578836, Verbindung
Reaktionsgleichung
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C@H:6]2[O:8][CH2:7]2)=[CH:4][CH:3]=1.[CH3:11][NH:12][CH2:13][CH2:14][OH:15]>>[ClH:1].[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C@@H:6]([OH:8])[CH2:7][N:12]([CH2:13][CH2:14][OH:15])[CH3:11])=[CH:4][CH:3]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
To (R)-4-chloro-styrene oxide (1.55 g, 10.0 mmol), N-methyl ethanolamine (788 mg, 1.05 equivalents) was added; and the mixture was stirred at 100° C. for 15 hours. The mixture was cooled to room temperature to obtain the reaction mixture of the title compound (chemical purity: 79.8 area %, N-methyl ethanolamine: 0.5 area %, 5.4 area % of regioisomer was contaminated). To the reaction mixture, 28 wt % hydrogen chloride solution in isopropanol (1.55 g, 1.2 equivalents) was added, and ethyl acetate (25 mL) was added dropwise thereto; as a result, crystals were precipitated. After the mixture was stirred at 25° C. for 17 hours, the crystals were separated by filtration under reduced pressure. The crystals were washed with ethyl acetate (10 mL), and dried under vacuum, to obtain 2.26 g of the title compound as white crystals (yield: 78%, chemical purity: 91.5 area %, N-methyl ethanolamine was not detected, 3.6 area % of regioisomer was contaminated). The retention time in the chemical purity analysis method was 1.8 min.