Dimethyl Disulfide → HCID 22678482, compound

Temperature

0 °C

1.05 g of 1-[(ethoxymethoxy)methyl]-3,4-methylenedioxybenzene was dissolved in 10 ml of diethyl ether, 2 ml of a 2.52 M n-butyllithium hexane solution was added thereto at 0° C., and the mixture was stirred for 2 hours, and then 471 mg of methyldisulfide was added dropwise at −70° C. After completing the dropwise addition, the mixture was further stirred at room temperature for 12 hours. A 1N aqueous sodium hydroxide was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified by silica gel column chromatography (ethyl acetate:hexane=1:20), to give 561 mg of the title compound as a colorless oil.

1. additionthe dropwise addition
2. stirringthe mixture was further stirred at room temperature for 12 hours
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated
7. customthe crude product was purified by silica gel column chromatography (ethyl acetate:hexane=1:20)

ORD record

ord-073fa60270c64157bf7dd9d4aba3a970

Source dataset

uspto-grants-2004_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06784192B2