反应详情

温度

0 °C

A solution of 4-([4-2-butynyloxy)phenyl]sulfonyl}-morpholine-3-carboxylic acid, methyl ester (0.1 g, 0.28 mmol) in 2.4 mL of THF:methanol:water [4:1:1] was cooled in an ice bath and 2N LiOH (0.3 mL, 0.59 mmol) was added. The reaction was stirred at 0° C. for 30 minutes and at room temperature for 2 hours. After evaporating the solvent, the residue was diluted with ether and filtered. The solid was dissolved in water, neutralized with 1N HCl to pH˜3 and extracted with dichloromethane. The organic layer was washed with water and brine, dried over sodium sulfate, filtered and concentrated to give 0.06 g of 4-[4-(2-butynyloxy)phenyl]sulfonyl}-morpholine-3-carboxylic acid. Yield˜69.8%. mp 40-42° C. Electrospray Mass Spec 338.1(M−H)−.

1. customAfter evaporating the solvent
2. additionthe residue was diluted with ether
3. filtrationfiltered
4. dissolutionThe solid was dissolved in water
5. extractionextracted with dichloromethane
6. washThe organic layer was washed with water and brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated