反应 #432318

ord-5c393ffbbf5f4ea1ae77778299073b47

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The reaction mixture was washed with a diluted hydrochloric acid, water
  2. 2
    干燥an aqueous solution saturated with sodium bicarbonate, water and an aqueous soluction saturated with sodium chloride in this order, then dried with anhydrous sodium sulfate
  3. 3
    其他The solvent was removed by evaporation
  4. 4
    其他the residue thus obtained
  5. 5
    workup.ADDITIONwas added
  6. 6
    其他thereto form a hydrochlodide

实验过程

To a solution containing 1.77 g of 1-amino-2,3-dihydro-4,6-dimethyl-7-hydroxy-1H-indene and 2 ml of triethylamine in 100 ml of chloroform was added dropwise 2.23 g of octyl chloride at room temperature. Then the reaction micture was stirred at the same temperature for 4 hours. The reaction mixture was washed with a diluted hydrochloric acid, water, an aqueous solution saturated with sodium bicarbonate, water and an aqueous soluction saturated with sodium chloride in this order, then dried with anhydrous sodium sulfate. The solvent was removed by evaporation and the residue thus obtained was dissolved in ethanol, tna an ethanol saturated with hydrogen chloride gas was added thereto form a hydrochlodide. Recrysttallized form acetonitrile to obtain 0.49 g of 2,3-dihydro-1-octylamino-4,6-dimethyl-7-hydroxy-1H-indene hydrochloride. Colorless needle-like crystals. Melting point: 120°-121° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05055474uspto-grants-1991_10