Dimethylformamide dimethyl acetal → HCID 178526359, compound

To a solution of 4-(chloromethyl)pyridin-2-amine (4-1) (1.56 g, 8.7 mmol) in propan-2-ol (15 mL) was added DMF-DMA (1.56 mL, 11.3 mmol) at room temperature under N2. The reaction mixture was heated to 90° C. for 3 h. After cooled to 50° C., the mixture was treated with NH2OH.HCl (0.781 g, 11.3 mmol), then stirred at 50° C. overnight. After cooled to room temperature, the mixture was concentrated and purified by chromatography on silica gel to afford the title compound (820 mg). MS (m/z): 186 (M+1)+.

1. temperatureAfter cooled to 50° C.
2. temperatureAfter cooled to room temperature
3. concentrationthe mixture was concentrated
4. custompurified by chromatography on silica gel

ORD record

ord-807fcd1429d04fc2b39b3fa6cf263654

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08987269B2