反应详情

温度

80 °C

To a solution of (4-[(phenylmethyl)oxy]-5-{[(trifluoromethyl)sulfonyl]oxy}-2-pyridinyl)methyl acetate (12.15 g, 30 mmol) in toluene (500 ml) was added (R)-(+)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.87 g, 3 mmol). The reaction mixture was purged with argon. Palladium acetate (663 mg, 3 mmol) was added and the mixture was stirred for 10 minutes. 2-Methyl-2-propanethiol sodium salt (4.69, 41.8 mmol) was added and the reaction mixture was flushed again with argon then heated to 80° C. for 7 hours then cooled. The solvent was evaporated. The residue was partitioned between a 1:1 mixture of water and EtOAc. The organic layer was separated and washed with brine, dried over magnesium sulphate and filtered through Kieselguhr. The residue was chromatographed eluting with s 4:1 mixture of hexane:EtOAc affording the product (8.3 g, 80%).

1. customThe reaction mixture was purged with argon
2. customthe reaction mixture was flushed again with argon
3. temperaturethen cooled
4. customThe solvent was evaporated
5. customThe residue was partitioned between a 1:1 mixture of water and EtOAc
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried over magnesium sulphate
9. filtrationfiltered through Kieselguhr
10. customThe residue was chromatographed
11. washeluting with s 4:1 mixture of hexane