反应详情

温度

0 °C

To a stirred solution of oxalyl chloride (47.8 ml, 0.545 mol) at 0° C. in 240 mL of CH2Cl2 was added a DMF (43.0 ml) solution of 4-but-2-ynyloxy-benzenesulfonic acid sodium salt in a drop wise manner. The reaction mixture was stirred at 0° C. for 30 min and then let warm to room temperature and stirred for 18 h. The reaction was then poured into ice and extracted with hexanes. The organics were washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo to provide 42.0 g (95%) of the desired product as yellow solid.

1. temperaturelet warm to room temperature
2. stirringstirred for 18 h
3. additionThe reaction was then poured into ice
4. extractionextracted with hexanes
5. washThe organics were washed with water and brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo