反应详情

In a round-bottom flask maintained under an inert atmosphere, 4.72 mL (38.8 mmoles) of 2-methoxythiophenol, 10.72 g (77.6 mmoles) of potassium carbonate, 5.13 g of diluted methyl (2R)-2-methyl-3-[(methylsulfonyl)oxy]propanoate (6a-1) and 100 mL of anhydrous THF then 329 mg (0.97 mmole) of tetrabutylammonium hydrogen sulfate are introduced. The reaction medium is brought to 60° C. for 24 h under vigorous stirring then concentrated under reduced pressure. The residue is taken up with water and is extracted with ethylic ether. The combined organic phases are washed with a 1 N soda solution, water, brine, then dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue is taken up in methanol and concentrated then taken up again in methanol (10 mL/1 g of residue). The bis(methoxyphenyl) disulfide [13920-94-0] that slowly precipitates is eliminated by filtration. The filtrate is evaporated under reduced pressure to yield the title compound in the form of a pale yellow oil (6.4 g, 26.6 mmoles).

1. concentrationthen concentrated under reduced pressure
2. extractionis extracted with ethylic ether
3. washThe combined organic phases are washed with a 1 N soda solution, water, brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. concentrationconcentrated
8. customThe bis(methoxyphenyl) disulfide [13920-94-0] that slowly precipitates
9. filtrationis eliminated by filtration
10. customThe filtrate is evaporated under reduced pressure