反应详情

Sodium hydride (60% in mineral oil, 360 mg, 9.00 mmol) is added in portions to a mixture of 3-(3-(trifluoromethyl)phenylamino)cyclopent-2-enone (2.16 g, 8.96 mmol) and 2-methyltetrahydrofuran (30 mL). After 30 min tert-butyl (2-bromo-4-cyanophenyl)(phenyl-sulfonyl)methylcarbamate (Step 1, 3.35 g, 7.43 mmol) is added and the mixture is stirred at room temperature for 2 h. Water is added and the phases are separated. The aqueous phase is extracted twice with ethyl acetate, and the combined organic phases are washed with water, dried over MgSO4 and concentrated under reduced pressure. The residue is treated with tert-butyl methyl ether, and the mixture is stirred for 15 min. The precipitate is filtered, washed with tert-butyl methyl ether, and dried. Yield: 3.18 g. ESI mass spectrum: [(79Br)-M+H]+=550, [(81Br)-M+H]+=552; Retention time HPLC: 0.73 min (X012_S01).

1. customthe phases are separated
2. extractionThe aqueous phase is extracted twice with ethyl acetate
3. washthe combined organic phases are washed with water
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure
6. additionThe residue is treated with tert-butyl methyl ether
7. stirringthe mixture is stirred for 15 min
8. filtrationThe precipitate is filtered
9. washwashed with tert-butyl methyl ether
10. customdried
11. custom0.73 min (X012_S01)