反応 #432318

反応方程式

hydrogen chloride

1-amino-2,3-dihydro-4,6-dimethyl-7-hydroxy-1H-indene

triethylamine

octyl chloride

→

2,3-dihydro-1-octylamino-4,6-dimethyl-7-hydroxy-1H-indene hydrochloride

収率 15.1%

溶媒

chloroform

ethanol

ethanol

acetonitrile

反応条件

後処理

1. 1
   洗浄The reaction mixture was washed with a diluted hydrochloric acid, water
2. 2
   乾燥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
   その他The solvent was removed by evaporation
4. 4
   その他the residue thus obtained
5. 5
   workup.ADDITIONwas added
6. 6
   その他thereto form a hydrochlodide

実験手順

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.

出典