تفاعل #44171

معادلة التفاعل

Methanesulfonyl chloride

2-(3-iodophenyl)ethanol

diisopropylethylamine

→

title compound

المردود 45.0%

2-(3-Iodophenyl)ethyl methanesulfonate

المردود 45.0%

المذيبات

dichloromethane

ammonium chloride

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with dichloromethane
2. 2
   غسيلwashed with aqueous sodium hydrogencarbonate solution, brine
3. 3
   تجفيفdried over sodium sulfate
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   أخرىThe crude was purified

الإجراء التجريبي

Methanesulfonyl chloride (1.5 mL, 1.2 eq.) was added dropwise to a stirred solution of 2-(3-iodophenyl)ethanol (3.6 g) in dichloromethane (100 mL) and diisopropylethylamine (3.8 mL, 1.5 equiv.) at 0° C. The solution was warmed to room temperature and stirred for 18 h. The reaction mixture was diluted with aqueous ammonium chloride solution and extracted with dichloromethane. The organic layers were combined, washed with aqueous sodium hydrogencarbonate solution, brine, dried over sodium sulfate and concentrated under reduced pressure. The crude was purified using column chromatography (SiO2 cartridge) using DCM-cyclohexane (70:30) to afford the title compound (3.2 g, 45% yield).

المصدر