반응 #1286511

반응 방정식

intermediate A

5-hexylsulfonamido-2-methylbenzoxazole

ethyl p-toluenesulfonate

diethyl ether

→

3-ethyl-5-hexylsulfonamido-2-methylbenzoxazolium p-toluenesulfonate

용매

methanol

반응 조건

후처리

1. 1
   온도Upon cooling to room temperature
2. 2
   온도The solid precipitate was chilled at 2° C. overnight
3. 3
   여과filtered
4. 4
   세척The tan powder was thoroughly washed with ether
5. 5
   기타recrystallized from 200 ml hot isopropyl alcohol

실험 절차

A mixture of 60 g of intermediate A and 44 g ethyl p-toluenesulfonate was heated in a round bottom flask at 150° C. for 5 minutes. Upon cooling to room temperature, the crude brown mass was almost solidified. The product was dissolved in 25 ml methanol and poured into 300 ml diethyl ether with rapid stirring for 1 hour. The solid precipitate was chilled at 2° C. overnight, and then filtered. The tan powder was thoroughly washed with ether and recrystallized from 200 ml hot isopropyl alcohol to yield 23.4 g of 3-ethyl-5-hexylsulfonamido-2-methylbenzoxazolium p-toluenesulfonate (Intermediate B).

출처