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A mixture of methyl chloroformate (25.0 g), sulfuryl chloride (35.7 g) and α,α'-azobis(isobutyronitrile) (100 mg) is refluxed for 8 hours. After cooling, the reaction mixture is diluted with hexane (150 ml) and 3-pentanol (24.0 g) is added thereto. Pyridine (42.0 g) is added dropwise to the mixture for 20 minutes under ice-cooling and stirring. After the mixture is stirred at room temperature overnight, hexane (200 ml) is added thereto. The reaction mixture is washed with water, dried, filtered and evaporated to remove the solvent. The residue is distilled under reduced pressure to give 3-pentyloxycarbonyloxymethyl chloride (26.3 g).

1. temperatureis refluxed for 8 hours
2. temperatureAfter cooling
3. additionis added
4. temperaturecooling
5. stirringAfter the mixture is stirred at room temperature overnight
6. washThe reaction mixture is washed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customto remove the solvent
11. distillationThe residue is distilled under reduced pressure