Methanol → Methoxysalicylic Acid

Temperatur

85 °C

To a first solution of 1.19 grams (0.03 mole) of NaOH in 50 milliliters of water were added 5 grams (0.03 mole) of 5-methoxysalicylic acid. The resulting mixture was heated to about 85° C. to help dissolve the acid. A second solution was prepared by dissolving 2.51 grams (0.015 moles) of manganese sulfate monohydrate in 25 milliliters of warm tap water. The manganese sulfate solution was added dropwise (fast drip) with stirring to the heated first solution containing the sodium salt of the acid. No precipitate was formed. When the addition was completed, the reaction mixture was stirred an additional 10 to 20 minutes at 85° C. and then cooled to room temperature, about 25° C. The reaction mixture was then dripped into 3 times the volume of methanol (about 225 milliliters), at which time a precipitate was formed. This solid product was collected, and washed with methanol. The product, manganese complex of methoxysalicylic acid, was dried in a vacuum oven at 120° F. to a constant weight to afford 2.01 grams (0.005 mole; 34 percent of theory) of an off white powder product.

1. dissolutionto help dissolve the acid
2. customA second solution was prepared
3. customNo precipitate was formed
4. additionWhen the addition
5. stirringthe reaction mixture was stirred an additional 10 to 20 minutes at 85° C.
6. temperaturecooled to room temperature, about 25° C
7. customat which time a precipitate was formed
8. customThis solid product was collected
9. washwashed with methanol
10. dry with materialThe product, manganese complex of methoxysalicylic acid, was dried in a vacuum oven at 120° F. to a constant weight
11. customto afford 2.01 grams (0.005 mole; 34 percent of theory) of an off white powder product

ORD-Eintrag

ord-c323dd8af5ae4538bb4c15b7c4ee5f78

Quelldatensatz

uspto-grants-1995_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05393632