Hydrochloric Acid → Ethyl 3,4-Diaminobenzoate

One mole (152 g.) of 3,4-diaminobenzoic acid was stirred with 2 liters of ethanol in a Morton flask. Hydrogen chloride gas was passed through the stirred suspension for about 2 hours. As the gas was absorbed, the slurry became gel-like in character. Ethanol (500 ml.) was added to the reaction mixture to disperse the gel. The reaction mixture was refluxed 24 hours. The mixture was filtered and the filtrate was evaporated to dryness in vacuo. The filter cake and the filtrate residue were dissolved in 9 liters of water. The aqueous solution was made basic by the addition of solid sodium carbonate. The product precipitated from the basic solution. The material was filtered and dried to yield 130 grams of ethyl 3,4-diaminobenzoate.

1. customAs the gas was absorbed
2. additionEthanol (500 ml.) was added to the reaction mixture
3. additionto disperse the gel
4. temperatureThe reaction mixture was refluxed 24 hours
5. filtrationThe mixture was filtered
6. customthe filtrate was evaporated to dryness in vacuo
7. dissolutionThe filter cake and the filtrate residue were dissolved in 9 liters of water
8. additionThe aqueous solution was made basic by the addition of solid sodium carbonate
9. customThe product precipitated from the basic solution
10. filtrationThe material was filtered
11. customdried

ORD-Eintrag

ord-f567241d11dc4f189a4f53556ab9f2cd

Quelldatensatz

uspto-grants-1977_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04018790