Water → HCID 178511560, Verbindung

Temperatur

0 °C

To a stirred suspension of trans-4-aminocyclohexanecarboxylic acid hydrochloride (0.5 g, 2.8 mmol) in anhydrous THF (10 mL) at 0° C. under argon was added dropwise lithium aluminum hydride (2 M solution in THF, 5.6 mL, 11 mmol). The mixture was stirred for 1 h at 0° C., then allowed to warm to rt and stir for an additional 1 h. The mixture was then heated in a sealed tube at 85° C. for 12 h. The mixture was cooled to 0° C. and H2O (600 μL) was slowly added, followed by a 1 M aq NaOH (1.2 mL) and H2O (1.8 mL). The mixture was diluted with CH2Cl2 (50 mL) and stirred for 30 min at rt. The mixture was filtered, and the filtrate was concentrated under reduced pressure to afford (trans-4-aminocyclohexyl)methanol (323 mg, 90%) as a white solid that did not require further purification.

1. temperatureto warm to rt
2. stirringstir for an additional 1 h
3. temperatureThe mixture was then heated in a sealed tube at 85° C. for 12 h
4. temperatureThe mixture was cooled to 0° C.
5. stirringstirred for 30 min at rt
6. filtrationThe mixture was filtered
7. concentrationthe filtrate was concentrated under reduced pressure

ORD-Eintrag

ord-f8187e0320f94933b8ec7f9f88e0de1d

Quelldatensatz

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08952058B2