反应详情

Formic acid (3.0 mL, 79 mmol) is added to a solution of tert-butyl carbamate (1.436 g, 12.3 mmol), 4-formyl-3-methylsulfanyl-benzonitrile (INTERMEDIATE 1; 1.975 g, 11.1 mmol) and sodium benzenesulfinate (2.012 g, 12.2 mmol) in a mixture of THF (3.0 mL) and water (7 mL), and the mixture is stirred at room temperature for 3 days. Water is added, the precipitate is filtered off and washed with water. The precipitate is treated with tert-butyl methyl ether, and the mixture is stirred for 30 min. The precipitate is filtered off, washed with tert-butyl methyl ether and dried. Yield: 3.5 g.

1. filtrationthe precipitate is filtered off
2. washwashed with water
3. additionThe precipitate is treated with tert-butyl methyl ether
4. stirringthe mixture is stirred for 30 min
5. filtrationThe precipitate is filtered off
6. washwashed with tert-butyl methyl ether
7. customdried