Hydrochloric Acid → HCID 13748797, compound

To a suspension of iron powder (135.4 g) in water (140 ml), with vigorous stirring at 50°-60° C., was slowly added concentrated hydrochloric acid (18 ml). After ethanol (350 ml) was mixed, 3-bromo-2,4-dichloro-5-fluoronitrobenzene (218.8 g) was added portionwise to the suspension at 52°-76° C. during an hour. After stirring for 75 minutes at the same temperature, the hot reaction mixture was filtered after adding benzene (500 ml) and the insoluble material was successively washed with hot ethanol (100 ml) and benzene (200 ml). The filtrate and washings were combined. The organic layers were washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and then concentrated. The resulting residue was recrystallized from ethanol-water to give the title compound (141.6 g) as light brown needles, mp 126°-129.5° C.

1. stirringAfter stirring for 75 minutes at the same temperature
2. filtrationthe hot reaction mixture was filtered
3. additionafter adding benzene (500 ml)
4. washthe insoluble material was successively washed with hot ethanol (100 ml) and benzene (200 ml)
5. washThe organic layers were washed with water saturated with sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. customThe resulting residue was recrystallized from ethanol-water

ORD record

ord-4d07673edfc54c26b71ae4d7adff89bf

Source dataset

uspto-grants-1989_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04826982