Hydrochloric Acid → HCID 14693075, Verbindung

A solution of 3-phenyl-4-hydroxybenzoic acid (131.1 g, 0.061 mole) and a 50 weight percent aqueous solution of NaOH (10.5 g, 0.131 mole) in 350 ml of deionized water was added to a 500 ml, three-necked, round-bottom flask equipped with a thermometer and a polytetrafluoroethylene-coated magnetic stir bar. The solution was stirred to homogeneity and then immersed in an ice water bath. With the solution temperature at 10° C., acetic anhydride (12.7 g, 0.124 mole) was added rapidly with stirring. Immediately, a white precipitate began to form. The reaction mixture was stirred for one hour at 10° C., then neutralized with concentrated HCl. The precipitate was filtered, washed in 500 ml of deionized water for one hour, filtered, and dried in an 80° C. vacuum oven for three hours yielding an off-white solid. The solid was recrystallized from a toluene and hexane mixture to give a fluffy white solid, 3-phenyl-4-acetoxybenzoic acid with a m.p. of 185° C. to 187° C.

1. customthree-necked, round-bottom flask equipped with a thermometer and a polytetrafluoroethylene-coated magnetic stir bar
2. customimmersed in an ice water bath
3. stirringwith stirring
4. customto form
5. stirringThe reaction mixture was stirred for one hour at 10° C.
6. filtrationThe precipitate was filtered
7. washwashed in 500 ml of deionized water for one hour
8. filtrationfiltered
9. customdried in an 80° C. vacuum oven for three hours
10. customyielding an off-white solid
11. customThe solid was recrystallized from a toluene and hexane mixture

ORD-Eintrag

ord-d646333144384e0490ed2df99df02e64

Quelldatensatz

uspto-grants-1993_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05268443