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HRID 655107作成日:2026年10月26日

Oxygen → Coolact HK

https://huagongshe.com/reaction/655107

反応式

関与物質

役割名称HCID仕込み量
反応物OxygenHCID 977—
反応物Sodium SulfiteHCID 24437—
反応物OzoneHCID 24823—
反応物(-)-IsopulegolHCID 170833—
溶媒MethanolHCID 887—
生成物Coolact HKHCID 1096476074.9%

反応手順

To a 500 ml reaction vessel, 70.0 g (453.8 mmol) of isopulegol and 140 ml of methanol were added and ozone generated in an oxygen stream by silent discharge was introduced into the reaction solution while the temperature of the solution was being kept between from 15° C. to 23° C. After 10 hours, disappearance of the raw material, isopulegol was confirmed by the gas chromatogram. The reaction solution obtained was cooled in an ice bath and then added into an excess amount of an aqueous sodium sulfite solution at a temperature of 30° C. or lower, followed by stirring for 2 hours. The solution was extracted with toluene. The toluene solution obtained was sequentially washed with dilute hydrochloric acid, an aqueous sodium carbonate solution, an aqueous ammonium chloride solution and brine, and was dried over anhydrous sodium sulfate. After filtration, the solvent was removed by evaporation under a reduced pressure. The mixture obtained was crystallized by adding 350 ml of heptane, and the crystal obtained was washed with 50 ml of cold heptane followed by drying under vacuum to obtain 53.08 g (yield: 74.9%) of the titled compound as a colorless needle crystal.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08071531B2
出典データセットuspto-grants-2011_12
ORD IDord-ea908ce9077e460aa44ebf1811bde07a
出典メモuspto-grants-2011_12