반응 #8381

반응 방정식

sodium hydroxide

3-methyl-3-oxetanemethanol

p-toluenesulfonyl chloride

water

→

3-METHYL-3-TOSYLMETHYLOXETANE

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added over 1 hour
2. 2
   기타A white precipitate formed immediately
3. 3
   기타The dichloromethane solution layer was then removed
4. 4
   건조dried with sodium sulfate
5. 5
   기타the solvent was removed

실험 절차

3-methyl-3-oxetanemethanol (100 g, 0.98 mol) was dissolved in 250 mL methylene chloride, and a 35% solution of sodium hydroxide (143.60 g, 1.08 mol)was added, and the reaction was cooled to 0° C. A solution of p-toluenesulfonyl chloride was added (186.67 g, 0.98 mol) in 375 mL methylene chloride was added over 1 hour. A white precipitate formed immediately. The reaction was stirred for 10 additional hours. 1000 mL of water was added. The dichloromethane solution layer was then removed, and dried with sodium sulfate, and the solvent was removed. Yield: 217.77 grams of 3-methyl-3-tosylmethyloxetane as white crystals, 87%.

출처