تفاعل #2304289

معادلة التفاعل

3-ethyl-3-hydroxymethyloxetane

p-toluenesulfonyl chloride

→

3-[(tosyloxy)methyl]-3-ethyloxetane

المردود 90.2%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added to it intermittently
2. 2
   workup.STIRRINGKept at 0° C., this was stirred for 5 hours
3. 3
   استخلاصThis was extracted with 500 ml of diethyl ether
4. 4
   غسيلThe diethyl ether layer was washed with 3% hydrochloric acid until its pH
5. 5
   غسيلwashed with saturated sodium carbonate solution and water in this order
6. 6
   تجفيفdried with anhydrous magnesium sulfate
7. 7
   أخرىThe solvent was evaporated away

الإجراء التجريبي

116 g of 3-ethyl-3-hydroxymethyloxetane (Toa Gosei's trade name, OXT-101) was added to 500 ml of pyridine, and cooled to 0° C. with stirring. 190 g of p-toluenesulfonyl chloride divided into a few portions was added to it intermittently. Kept at 0° C., this was stirred for 5 hours, and then 1 L of ice-water was poured into the reaction mixture. This was extracted with 500 ml of diethyl ether. The diethyl ether layer was washed with 3% hydrochloric acid until its pH became acidic, and then washed with saturated sodium carbonate solution and water in this order, and thereafter dried with anhydrous magnesium sulfate. The solvent was evaporated away, and 243 g of 3-[(tosyloxy)methyl]-3-ethyloxetane was obtained.

المصدر