反応 #5455

反応方程式

compound

3-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

p-methoxybenzyl chloride

triethylamine

sodium iodide

→

title compound

収率 32.4%

3-(4- Methoxybenzyloxycarbonyl)-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

収率 32.4%

溶媒

chloroform

反応条件

後処理

1. 1
   抽出extracted with dichloromethane
2. 2
   洗浄The organic layer was washed with water and with saturated saline solution
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by means of silica gel column chromatography (CHCl3)

実験手順

To a suspension of 50 mg (0.163 mmol) of the compound of Example 112 in 0.2 ml of chloroform were added 30.7 mg (0.196 mmol) of p-methoxybenzyl chloride, 16.5 mg (0.163 mmol) of triethylamine and 29.4 mg (0.196 mmol) of sodium iodide, and the mixture was stirred for 5 hours at room temperature, which was poured into ice-water and extracted with dichloromethane. The organic layer was washed with water and with saturated saline solution, dried over anhydrous sodium sulfate and concentrated. The residue was purified by means of silica gel column chromatography (CHCl3) to obtain 22.5 mg (0.0528 mmol) of title compound (yield 32%).

出典