Pyridine → 2-Methoxypropyl 4-methylbenzenesulfonate

To dichloromethane (30 mL) mixture of 2-methoxypropan-1-ol (1.6 g, 17.8 mmol) and pyridine (20.0 mL), was added p-toluenesulfonyl chloride (4.07 g, 21.4 mmol) while stirring on ice, and the mixture was stirred at room temperature for five hours. To the mixture, were added water and ethyl acetate. After thoroughly shaking the mixture, the organic layer was separated, and the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The mixture was filtered, and the solvent in the filtrate was then distilled off under reduced pressure. The residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate: n-heptane/ethyl acetate=2/1) to obtain the title compound (3.12 g, 12.8 mmol).

1. stirringthe mixture was stirred at room temperature for five hours
2. stirringAfter thoroughly shaking the mixture
3. customthe organic layer was separated
4. washthe organic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe mixture was filtered
7. distillationthe solvent in the filtrate was then distilled off under reduced pressure
8. customThe residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate

ORDレコード

ord-a871361464a84328b4e7488902f129ec

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08530504B2