Reaktionsgleichung
[CH3:1][C:2]1([CH2:12][O:13]CC#C)[NH:6][C:5]2(CCC[CH2:8][CH2:7]2)[O:4][CH2:3]1.Cl>O>[NH2:6][C:2]([CH3:1])([CH2:3][O:4][CH2:5][C:7]#[CH:8])[CH2:12][OH:13]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3-Methyl-3-prop-2-ynyloxymethyl-1-oxa-4-aza-spiro[4.5]decane (1.83 g) in an aqueous solution of HCl (6N) (2.73 ml) were refluxed for 1 hr. The reaction mixture was cooled down to room temperature, diluted with water and extracted thrice with ethyl ether. The two layers were separated. The aqueous layer was concentrated under reduced pressure to yield 2-amino-2-methyl-3-prop-2-ynyloxy-propan-1-ol hydrochloric salt (1.205 g) as a white beige solid which was used as such in Stage 3 described below. 1H NMR (DMSO) δ ppm: 8.02 (3H, s br); 5.47 (1H, s br); 4.21 (2H, s); 3.54-3.49 (5H, m); 1.15 (3H, s).
Aufarbeitung
- extractionextracted thrice with ethyl ether
- customThe two layers were separated
- concentrationThe aqueous layer was concentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-ae3bb24121ea4854a6d21cbb4a62e16d
- Quelldatensatz
- uspto-grants-2013_04
- Patentnummer
- US08415272B2
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