Triethylamine → 229007-16-3

In 1,2-dichloroethane (35 ml) were suspended 4-methylcyclohexanone (2.5 g), methylamine hydrochloride (1.6 g) and triethylamine (3.3 ml), and to the suspension was added sodium triacetoxy boron hydride (6.6 g) under ice-cooling. The mixture was stirred under nitrogen atmosphere at room temperature overnight. The solvent was evaporated, and the residue was neutralized with sodium hydroxide. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated. To the residue was added. 4N hydrochloric acid-ethyl acetate, and the solvent was evaporated to give N, 4-dimethyl-cyclohexylamine hydrochloride (2.6 g) as colorless crystals.

1. temperaturecooling
2. customThe solvent was evaporated
3. extractionThe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with saturated sodium chloride solution
5. dry with materialdried with anhydrous magnesium sulfate
6. customUnder reduced pressure, the solvent was evaporated
7. additionTo the residue was added
8. custom4N hydrochloric acid-ethyl acetate, and the solvent was evaporated

ORD record

ord-2aacd2acb9d846d0886cecfc85591a84

Source dataset

uspto-grants-2002_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06413947B1