反应详情

Thionyl chloride (5 ml.) was added dropwise to a stirred solution of 1.27 g. of 1,3-diacetyl-2-{4-[1-hydroxy-1-methyl)ethyl]-3-pyridyl}-5-(3-methyl-2-octyl)resorcinol in 40 ml. of pyridine, cooled in an ice-salt bath at -10°. The mixture was stirred and the temperature was allowed to rise to 0° within 11/2 hours. The mixture was poured into ice water and was extracted with ether. The ether extracts were washed with water, dried over anhydrous sodium sulfate, and evaporated in vacuo. The residue was chromatographed on a Florisil column (60-100 mesh) using graded methanol/benzene solvent mixtures to give the pure product.

1. customto rise to 0° within 11
2. custom2 hours
3. extractionwas extracted with ether
4. washThe ether extracts were washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. customevaporated in vacuo
7. customThe residue was chromatographed on a Florisil column (60-100 mesh)
8. customto give the pure product