反応 #321871

反応方程式

N-(2-chloroethyl)-7-chloro-4-quinolinamine hydrochloride

water

sodium hydroxide

→

colourless crystals

収率 64.3%

(RS)-(7-Chloro-quinolin-4-yl)-[2-(3-methyl-piperidin-1-yl)-ethyl]-amine

収率 64.3%

溶媒

3-methylpiperidine

反応条件

後処理

1. 1
   抽出extracted three times with 50 ml of ethyl acetate each time
2. 2
   洗浄The combined extracts were washed with a small amount of water
3. 3
   濃縮concentrated
4. 4
   その他The residue was recrystallized from 80 ml of acetone

実験手順

2.5 g of N-(2-chloroethyl)-7-chloro-4-quinolinamine hydrochloride in 25 ml of 3-methylpiperidine were held at 100° C. in a sealed tube for 24 hours. Thereafter, 100 ml of water were added, the mixture is adjusted to pH 12 by means of concentrated sodium hydroxide solution and extracted three times with 50 ml of ethyl acetate each time. The combined extracts were washed with a small amount of water and concentrated. The residue was recrystallized from 80 ml of acetone. 0.88 g of colourless crystals, m.p.: 148°-151° C., was obtained.

出典