反应详情

To a solution of 167 (8.924 g, 32.5 mmol) in THF was added methyl thioglycolate (4.36 mL, 48.8 mmol) and stirred 2 hours at room temperature. MAGNESIUM SULFATE (3.91 g, 32.5 mmol) was added and the reaction mixture was stirred for 1 hour. Then CESIUM CARBONATE (10.60 g, 32.5 mmol) in 30 mL of MeOH was added and stirred for an additional 2 hours at room temperature. The reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with brine, dried over sodium sulfate and filtered. The solvent was evaporated and the residue was purified by silica gel chromatography (0%-5% ethyl acetate in hexanes) to yield 168 in 54% (6.389 g) as an orange solid

1. stirringthe reaction mixture was stirred for 1 hour
2. stirringstirred for an additional 2 hours at room temperature
3. filtrationThe reaction mixture was filtered
4. concentrationthe filtrate was concentrated in vacuo
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed with brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customThe solvent was evaporated
10. customthe residue was purified by silica gel chromatography (0%-5% ethyl acetate in hexanes)