반응 #5455

반응 방정식

compound

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

p-methoxybenzyl chloride

triethylamine

sodium iodide

→

title compound

수율 32.4%

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

수율 32.4%

용매

chloroform

반응 조건

후처리

1. 1
   추출extracted with dichloromethane
2. 2
   세척The organic layer was washed with water and with saturated saline solution
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   농축concentrated
5. 5
   기타The residue was purified by means of silica gel column chromatography (CHCl3)

실험 절차

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%).

출처