反应详情

2-Chloro-5-(4-hydroxymethylpiperidinosulfonyl)benzoic acid (5.0 g.) is refluxed overnight with 50 ml. of thionyl chloride. After evaporation to dryness, the residue is dissolved in 70 ml. of acetone, 30 ml. of water added and the mixture is allowed to stand at room temperature for a half hour. The solution is then filtered and concentrated to half volume. On the addition of 20 ml. of water a precipitated oil is obtained which crystallizes on stirring. Recrystallization from acetone-benzene yields the product, m.p. 175°-177° C.

1. customAfter evaporation to dryness
2. dissolutionthe residue is dissolved in 70 ml
3. additionof water added
4. waitto stand at room temperature for a half hour
5. filtrationThe solution is then filtered
6. concentrationconcentrated to half volume
7. additionOn the addition of 20 ml
8. customof water a precipitated oil is obtained which
9. customcrystallizes
10. customRecrystallization from acetone-benzene
11. customyields the product, m.p. 175°-177° C.