2-Methyl-2-butanol → HCID 178526251, Verbindung

Temperatur

67 °C

A mixture of 2-chloropyridine-N-oxide (16.6 g, 100 mmoles), 3-amino-1-propanol (15.3 ml, 200 mmoles), NaHCO3 (42 g, 0.5 mole), and tert-amyl alcohol (100 ml) was heated to reflux. After 23 hours, the reaction was cooled, diluted with CH2Cl2 (300 ml), and filtered to remove insoluble materials. The filtrate was concentrated to afford a brown oil. The oil was dried under vacuum overnight. Ether (100 ml) was added to give a brown solid. The ether was decanted and the solid was washed further with ether/acetonitrile (3/1). The resulting solid was heated at 67° C. under vacuum to give the desired product (13.5 g). 1H NMR was consistent with the proposed structure.

1. temperaturewas heated to reflux
2. temperaturethe reaction was cooled
3. filtrationfiltered
4. customto remove insoluble materials
5. concentrationThe filtrate was concentrated
6. customto afford a brown oil
7. customThe oil was dried under vacuum overnight
8. additionEther (100 ml) was added
9. customto give a brown solid
10. customThe ether was decanted
11. washthe solid was washed further with ether/acetonitrile (3/1)

ORD-Eintrag

ord-7638cfb683b8452eb81dd8e69519514f

Quelldatensatz

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06949578B2