Triethylamine → 229007-16-3

In 1,2-dichloroethane (35 ml) were suspended 4-methyl-cyclohexanone (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 over night. 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 4 N 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 4 N hydrochloric acid-ethyl acetate
8. customthe solvent was evaporated

ORD record

ord-b5dc4e1d7fd348bf8218ef94202d14fc

Source dataset

uspto-grants-2001_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06172061B2