Hydrochloric Acid → 1-(5-amino-2-chlorophenyl)ethanone

5 g of solid 2-chloro-5-nitroacetophenone (see J. Am. Chem. Soc. 76, 5482 (1952)) are introduced in portions and with stirring at 65° C. to a mixture of 5.6 g of iron powder, 40 ml of ethanol, 9 ml of water and 1 ml of concentrated hydrochloric acid. Stirring of the reaction mixture is continued for 1 hour at 70° C. The mixture is allowed to cool to room temperature and then diluted with 300 ml of water, and a pH of 9 is established by adding 2N potassium carbonate solution. The mixture is filtered with suction through Celite, and the residue is washed with 200 ml of ethyl acetate. The filtrate is transferred to a separating funnel, and the aqueous phase is discarded. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated.

1. filtrationThe mixture is filtered with suction through Celite
2. washthe residue is washed with 200 ml of ethyl acetate
3. customThe filtrate is transferred to a separating funnel
4. washThe organic phase is washed with saturated sodium chloride solution
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated

ORD-Eintrag

ord-feb17e5f2234486982ff99672b9803eb

Quelldatensatz

uspto-grants-1994_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05336663