反应详情

Formic acid (3.9 mL, 104 mmol) is added to a solution of tert-butyl carbamate (1.90 g, 16.2 mmol), 2-bromo-4-cyanobenzaldehyde (3.41 g, 16.2 mmol) and sodium benzenesulfinate (2.67 g, 16.2 mmol) in a mixture of tetrahydrofuran (7.0 mL) and water (60 mL), and the mixture is stirred at room temperature for 6 days. Water (180 mL) is added, and the precipitate is filtered and washed with water. The precipitate is treated with tert-butyl methyl ether (30 mL), and the mixture is stirred for 30 min. The precipitate is filtered, washed with tert-butyl methyl ether, and dried. Yield: 3.35 g. ESI mass spectrum: [(79Br)-M+H]+=451, [(81Br)-M+H]+=453; Retention time HPLC: 0.66 min (X012_S01).

1. filtrationthe precipitate is filtered
2. washwashed with water
3. additionThe precipitate is treated with tert-butyl methyl ether (30 mL)
4. stirringthe mixture is stirred for 30 min
5. filtrationThe precipitate is filtered
6. washwashed with tert-butyl methyl ether
7. customdried
8. custom0.66 min (X012_S01)