Pyridine → HCID 11084789, compound

Glycerol formal (14 g) was dissolved in anhydrous ether (400 ml) and, after adding pyridine (15 g) at −10° C., a solution of chloromethyl chloroformate (25 g) in anhydrous ether (50 ml) was added dropwise over the period of 10 minutes. After the reaction solution was stirred at room temperature for 20 hours, the deposited pyridine hydrochloride was removed by filtration. The filtrate was washed with a saturated sodium chloride aqueous solution (400 ml×2), and then dried over anhydrous magnesium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by subjecting to silica gel chromatography (eluent: ethyl acetate/hexane=1/5→ethyl acetate/hexane=1/3) to obtain chloromethyl (1,3-dioxan-5-yl) carbonate (1.7 g) as a colorless oily product.

1. customthe deposited pyridine hydrochloride was removed by filtration
2. washThe filtrate was washed with a saturated sodium chloride aqueous solution (400 ml×2)
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe residue obtained
5. distillationby distilling off the solvent under reduced pressure
6. customwas purified

ORD record

ord-1224483b01e8404792d218f116f8286f

Source dataset

uspto-grants-2002_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06407129B1