Tin tetrachloride dihydrate → HCID 178418959, compound

Temperature

50 °C

A mixture of 5-bromo-3-nitropyridin-2-ol (1.26 g, 4.6 mmol) and tin chloride dihydrate (3.91 g, 17.3 mmol) in ethyl acetate (19.3 mL) was heated at 50° C. for 20 h. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (100 mL) and washed with brine. The aqueous layer was separated and extracted with ethyl acetate (5×50 mL). The combined organic layers were dried with sodium sulfate, filtered and concentrated in vacuo to give a black solid 580 mg (53%), which was used without further purification.

1. temperatureThe reaction mixture was cooled to room temperature
2. washwashed with brine
3. customThe aqueous layer was separated
4. extractionextracted with ethyl acetate (5×50 mL)
5. dry with materialThe combined organic layers were dried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo

ORD record

ord-e0a31bbd9a564ae0ad27fb43af393f71

Source dataset

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07087622B2