반응 #833528

반응 방정식

3-ethyl-3-hydroxymethyloxetane

pyridine

p-Toluene sulfonyl chloride

→

3-[(tosyloxy)methyl]3-ethyloxetane

용매

water

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring for 5 hours
2. 2
   기타while keeping at 0° C.
3. 3
   추출It was extracted with diethyl ether (500 mL)
4. 4
   세척were washed with water
5. 5
   세척Then, the extracts were washed with a saturated solution of sodium carbonate and water successively
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off

실험 절차

3-ethyl-3-hydroxymethyloxetane (trade name of product, OXT-101®, manufactured by To a Gosei Co.; 116 g) was added to pyridine (500 mL) and cooled to 0° C. while stirring. p-Toluene sulfonyl chloride (190 g) was added divisionally for several times. After stirring for 5 hours while keeping at 0° C., the reaction mixture was poured to iced water (1 L). It was extracted with diethyl ether (500 mL), the pH was rendered acidic with 3% hydrochloric acid, and extracts were washed with water. Then, the extracts were washed with a saturated solution of sodium carbonate and water successively and dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain 3-[(tosyloxy)methyl]3-ethyloxetane (243 g).

출처