反应详情

A solution of trans-4-[2-(6-bromopyridin-2-yl)-2-oxoethylcarbamoyl]cyclohexanecarboxylic acid methyl ester (7.38 g, 19.3 mmol) obtained in Step 2 and a Lawesson reagent (8.20 g, 20.3 mmol) in tetrahydrofuran (120 ml) was heated at reflux for 2 hours in an Ar stream. After the reaction solution was concentrated, a saturated aqueous sodium bicarbonate was added and extracted with ethyl acetate. The organic layer was washed with a saturated sodium bicarbonate aqueous solution and dried over magnesium sulfate, and after concentrated, the residue was purified by flash chromatography on silica gel (n-hexane:ethyl acetate=1:1) and the title compound (6.1 g) was obtained.

1. temperatureat reflux for 2 hours in an Ar stream
2. concentrationAfter the reaction solution was concentrated
3. additiona saturated aqueous sodium bicarbonate was added
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with a saturated sodium bicarbonate aqueous solution
6. dry with materialdried over magnesium sulfate
7. concentrationafter concentrated
8. customthe residue was purified by flash chromatography on silica gel (n-hexane:ethyl acetate=1:1)