HRID925102

反应详情

EQUATION

反应方程式

HRID 925102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

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%.

WORKUP

后处理

  1. customobtaining a mixture
  2. customThe reaction vessel was sealed
  3. customto obtain a reaction mixture
  4. customThereafter, the obtained reaction mixture
  5. temperaturewas cooled
  6. filtrationfiltered
  7. washThe obtained solid was washed with 20 parts by weight of 2-propanol
  8. customThe washing liquid recovered
  9. washafter washing
  10. customthe filtrate obtained by filtration
  11. concentrationThe combined mixture was concentrated under reduced pressure