Reacción #1012284

Ecuación de reacción

(3R)-1,1,3-trimethyl-4-aminoindane

→

1,1,3-trimethyl-4-aminoindane

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroobtaining a mixture
2. 2
   OtroThe reaction vessel was sealed
3. 3
   Otroto obtain a reaction mixture
4. 4
   OtroThereafter, the obtained reaction mixture
5. 5
   Temperaturawas cooled
6. 6
   Filtraciónfiltered
7. 7
   LavadoThe obtained solid was washed with 20 parts by weight of 2-propanol
8. 8
   OtroThe washing liquid recovered
9. 9
   Lavadoafter washing
10. 10
    Otrothe filtrate obtained by filtration
11. 11
    ConcentraciónThe combined mixture was concentrated under reduced pressure

Procedimiento

Into a reaction vessel were charged 6.00 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 96.5% ee) and 1.62 parts by weight of 5% palladium-carbon (STD-type, manufactured by N. E. Chemcat Corporation), thereby obtaining a mixture. The reaction vessel was sealed, the gas in the reaction vessel was replaced with nitrogen, and then the mixture was stirred at 200° C. for 7.5 hours to obtain a reaction mixture. Thereafter, the obtained reaction mixture was cooled and filtered. The obtained solid was washed with 20 parts by weight of 2-propanol. The washing liquid recovered after washing and the filtrate obtained by filtration were combined. The combined mixture was concentrated under reduced pressure to obtain 5.06 parts by weight of 1,1,3-trimethyl-4-aminoindane. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 3.3% ee and a recovery rate of 84.3%.

Fuente