1,1,3-Trimethyl-indan-4-ylamine hydrochloride synthesis

Yield:-

Reaction Conditions:

with hydrogenchloride in water;toluene at 70; for 1 h;Inert atmosphere;

Steps:

2

(0053) Under a nitrogen atmosphere, 158.5 g of a toluene solution containing crude 4-amino-1,1,3-trimethylindane (purity: 88.5%) (content: 25.2%), 41.8 g of toluene, and 18.0 g of water were added into a flask. The resultant mixture was heated to 70°C, and then thereto was added 36.5 g of concentrated hydrochloric acid. The resultant mixture was stirred at 70°C for 1 hour. The resultant mixture was allowed to stand still and a water phase and an organic phase in which 4-amino-1,1,3-trimethylindane hydrochloride was dissolved were separated. While the organic phase was stirred, the phase was cooled to 5°C to precipitate crystals of 4-amino-1,1,3-trimethylindane hydrochloride. The precipitated crystal was isolated by filtration to obtain 4-amino-1,1,3-trimethylindane hydrochloride. Melting point: 228 to 229°C. (0054) The collected 4-amino-1,1,3-trimethylindane hydrochloride was dissolved in hot water. To the resultant solution was added an aqueous sodium hydroxide solution. Toluene was added to the resultant mixture, and then the resultant organic phase was separated therefrom. The organic phase was washed with water, and then concentrated under a reduced pressure to yield 36.9 g of 4-amino-1,1,3-trimethylindane as a liquid of light brown color. Yield: 92.2%, purity: 99.8%.

References:

EP2940001,2015,A1 Location in patent:Paragraph 0053; 0054; 0055; 0056; 0057-0060; 0063-0064