反应详情

温度

0 °C

To a cooled (0° C.), stirred portion of 1-methoxy-3-morpholin-4-yl-benzene (1.08 g; 5.6 mmol) was added neat to chlorosulfonic acid (1.8 mL; 28 mmol) via pipette over 2 minutes under calcium sulfate-dried atmosphere. The resulting thick, red solution was allowed to warm to room temperature and stirred for 5 hours. The resulting solution was poured onto ice, then extracted with CH2Cl2 (3×50 mL). Combined organic layers then were washed with brine, dried (MgSO4), filtered and concentrated in vacuo to give the acid as a light green solid (0.31 g; 20%).

1. customdried atmosphere
2. temperatureto warm to room temperature
3. additionThe resulting solution was poured onto ice
4. extractionextracted with CH2Cl2 (3×50 mL)
5. washCombined organic layers then were washed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo