反应详情

温度

110 °C

7.5 grams (0.027 mole) of the product of Example 1 was caused to react with 3.79 grams of K2CO3 in the least amount of water along with 200 mls of DMF. To this mixture was added 5 drops of 18 crown-6-ether. Into this solution was added 5.79 grams (0.027 mole) of 2-bromoethane sulfonic acid sodium salt and the mixture heated to 110° C. for 3 hours. The solution was filtered and the filtrate was distilled at reduced pressure. The residual solid was dissolved in excess water and poured into conc. hydrochloric acid. The solid that precipitated was filtered and washed with water and then air dried. The recovered solid was recrystallized from acetonitrile to give 2.7 grams of a yellow solid which melted at 138°-140° C.

1. filtrationThe solution was filtered
2. distillationthe filtrate was distilled at reduced pressure
3. dissolutionThe residual solid was dissolved in excess water
4. additionpoured into conc. hydrochloric acid
5. customThe solid that precipitated
6. filtrationwas filtered
7. washwashed with water
8. customair dried
9. customThe recovered solid was recrystallized from acetonitrile