Hydrochloric Acid → HCID 86714471, compound

Temperature

0 °C

Into a 250-mL 4-necked round-bottom flask, was placed 4-(2,3-difluorophenoxy)-aniline (8.84 g, 39.96 mmol, 1.00 equiv), hydrogen chloride (10.14 g, 100.01 mmol, 2.50 equiv), and water (20 mL). A solution of NaNO2 (3.04 g, 44.06 mmol, 1.10 equiv) in water (10 mL) was added dropwise with stirring in portions at 0° C. The mixture was stirred at 0° C. for half an hour. To this was added urea (1 g, 16.65 mmol). The mixture was stirred at 0° C. for 20 min and poured into the solution of NaI (18 g, 120.00 mmol, 3.00 equiv) in water (20 mL) at room temperature. The resulting solution was stirred at room temperature for 1 h and then extracted with ethyl acetate. The organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum to give 10.5 g (79%) of 1,2-difluoro-3-(4-iodophenoxy)benzene as brown oil.

1. customInto a 250-mL 4-necked round-bottom flask, was placed
2. stirringThe mixture was stirred at 0° C. for half an hour
3. stirringThe mixture was stirred at 0° C. for 20 min
4. stirringThe resulting solution was stirred at room temperature for 1 h
5. extractionextracted with ethyl acetate
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum

ORD record

ord-ab0e48ee3e714b1fabe0823d49bb0ecd

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08962635B2