反応 #3367

反応方程式

8-mercapto-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2-yl-ethyl)-amide

triethylamine

iodine

→

title compound

収率 83.0%

2-[2-(2-Pyridinyl)ethyl]-[1,3]dioxolo[4,5-g]isothiazolo[4,5-c]quinolin-3(2H)-one

収率 83.0%

溶媒

methanol

methanol

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度at reflux for 2 hours
3. 3
   温度cooled
4. 4
   濃縮concentrated to an oil
5. 5
   その他the solid was collected
6. 6
   その他recrystallized in ethanol

実験手順

To 4.1 g (0.012 mol) of 8-mercapto-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2-yl-ethyl)-amide (from Preparation 34) and 5 mL (0.035 mol) of triethylamine in 750 mL of methanol was added 2.95 g (0.012 mol) of iodine in 100 mL of methanol. The mixture was heated at reflux for 2 hours, cooled, and then concentrated to an oil. The residue was slurried in water, and the solid was collected and recrystallized in ethanol to give 3.5 g of the title compound, mp 200°-201° C.

出典