Hydrochloric Acid → 2,6-Dichloropyridine-3,4-diamine

温度

95 °C

To a solution of 2,6-dichloro-3-nitropyridin-4-amine in ethanol (150 mL) was added iron powder (14.3 g, 0.255 mol), water (46 mL), and then concentrated HCl (28 mL). The reaction mixture was then stirred at 95° C. for 16 hours, cooled to room temperature, and neutralized. The precipitates were collected by filtration and dried in vacuo. The crude product was then treated with water (200 mL) and extracted with EtOAc (3×200 mL). The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated to afford 7.85 g of the title compound (86.5% yield).

1. temperaturecooled to room temperature
2. filtrationThe precipitates were collected by filtration
3. customdried in vacuo
4. additionThe crude product was then treated with water (200 mL)
5. extractionextracted with EtOAc (3×200 mL)
6. dry with materialThe combined extracts were dried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated

ORDレコード

ord-e7a3ccedbad14f8e928c8f02d0d5d9a6

出典データセット

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09434726B2