Nitric Acid → Propane, 1,2-dichloro-2-fluoro-3-nitro-

To a mixture of 86 ml of anhydrous, 100% strength nitric acid and 300 ml of anhydrous hydrofluoric acid were added dropwise at -10° C. in the course of 3 hours 111 g (1 mol) of 2,3-dichloropropene. The reaction was slightly exothermic. After the dropwise addition had ceased, stirring was continued for a further 1 hour at -10° C. Then the mixture was poured on to ice and extracted using dichloromethane. The organic phase was washed with sodium hydrogencarbonate solution, dried over sodium sulphate and concentrated using a rotary evaporator. The crude product was distilled under an oil pump vacuum. This gave 115.8 g (=63% of theory) of product having a boiling point of 48° to 50° C. at 0.07 mbar and a Refractive Index nD20 of 1.4578 (at 24° C.). The product was 95.7% pure.

1. additionAfter the dropwise addition
2. additionThen the mixture was poured on to ice
3. extractionextracted
4. washThe organic phase was washed with sodium hydrogencarbonate solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customa rotary evaporator
8. distillationThe crude product was distilled under an oil pump vacuum
9. customof 1.4578 (at 24° C.)

ORD record

ord-afec642ef1af4c7c96b1e22144e82fe1

Source dataset

uspto-grants-1992_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05124476