反应详情

To a solution of methyl 4-chloro-6-(hydroxymethyl)-2-pyridinecarboxylate (166 mg, Ref: Kittika et al., Tetrahedron, 44 (10), 2821, (1988)) in dry dichloromethane (3 ml) was added thionyl chloride (66 μl). The solution was stirred for 40 minutes. LC/MS indication reaction completion. Solvent was removed u.r.p. (under reduced pressure) to give a white solid. Toluene (˜2 ml) added then removed u.r.p. The residue was dried in vacuo to give a white solid. (175 mg, 97%). LC/MS [MH+]=220/222, Rt=2.51 min. Title compound obtained as the free base.

1. customLC/MS indication reaction completion
2. customSolvent was removed u.r.p
3. custom(under reduced pressure) to give a white solid
4. customthen removed u.r.p
5. customThe residue was dried in vacuo
6. customto give a white solid