반응 #537908

반응 방정식

2-Indanol

diisopropylethylamine

Methanesulfonyl chloride

dimethylaminopyridine

→

crystals

수율 78.0%

Methanesulfonic acid indan-2-yl ester

수율 78.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타Solution was evaporated
2. 2
   기타partitioned between ethyl acetate and water
3. 3
   기타the organic phase separated
4. 4
   세척This was washed with NaHCO3 (sat) and with citric acid solution (5%)
5. 5
   건조dried over MgSO4
6. 6
   농축The filtered solution was concentrated
7. 7
   기타the resultant solid recrystallized from isopropanol-EtOH (3:1)

실험 절차

2-Indanol (20.00 g, 149.5 mmol) and diisopropylethylamine (21.2 g, 164 mmol) was stirred in dichloromethane (300 mL) at 0° C. Methanesulfonyl chloride (18.78 g, 164 mmol) and dimethylaminopyridine (1.80 g) were added simultaneously and stirring continued at room temperature for 18 h. Solution was evaporated, partitioned between ethyl acetate and water, and the organic phase separated. This was washed with NaHCO3 (sat) and with citric acid solution (5%) and dried over MgSO4. The filtered solution was concentrated and the resultant solid recrystallized from isopropanol-EtOH (3:1) to give off-white crystals (24.6 g, 78%).

출처