Hydrochloric Acid → 2-Methyloxan-4-amine--hydrogen chloride (1/1)

To a flask having an inner volume of 500 ml, made of glass and equipped with a stirring device, a thermometer and a reflux condenser were charged 65.3 g (392 mmol) of 4-hydrazino-2-methyltetrahydropyran hydrochloride with a purity of 100% and synthesized in the same manner as in the above-mentioned (1), 18.0 g of developed Raney nickel, 120 ml of ethanol, 120 ml of water and 40 ml (320 mmol) of 8 mol/l aqueous sodium hydroxide solution, and the mixture was reacted at 75° C. for 24 hours under hydrogen atmosphere. After completion of the reaction, the reaction mixture was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. Then, 200 ml of n-butyl alcohol and 50 ml (600 mmol) of 12 mol/l hydrochloric acid were added to the concentrate, the resulting mixture was concentrated under reduced pressure to obtain 38.2 g (Isolation yield: 63%) of 4-amino-2-methyltetrahydropyran hydrochloride with a purity of 98% (areal percentage by gas chromatography) as white powder.

1. customTo a flask having
2. customequipped with a stirring device
3. customthe mixture was reacted at 75° C. for 24 hours under hydrogen atmosphere
4. customAfter completion of the reaction
5. filtrationfiltered
6. concentrationthe filtrate was concentrated under reduced pressure
7. concentrationthe resulting mixture was concentrated under reduced pressure

ORD-Eintrag

ord-74d67d71ec3045ada3536c462be1ee0c

Quelldatensatz

uspto-grants-2008_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07365215B2