反应详情

温度

60 °C

1-Pentanesulfonic acid, sodium salt (10 g, 57.5 mmol) was charged into a 250 ml round bottom flask (allow headroom). Thionyl chloride (20 mL) is added; gas evolves, and a while solid forms. The mixture is heated at 60° C. for 3 hours. The solvents are removed in vacuo; toluene is added and removed in vacuo to remove residue of SOCl2. The residue is partitioned between CH2Cl2 and ice water; the organic layer is dried over Na2SO4. The crude product is purified by distillation (bp 54-56° C. @ 0.5 mm Hg) to give a clear oil, 61% yield.

1. customThe solvents are removed in vacuo
2. additiontoluene is added
3. customremoved in vacuo
4. customto remove residue of SOCl2
5. customThe residue is partitioned between CH2Cl2 and ice water
6. dry with materialthe organic layer is dried over Na2SO4
7. distillationThe crude product is purified by distillation (bp 54-56° C. @ 0.5 mm Hg)
8. customto give a clear oil, 61% yield