Hydrochloric Acid → HCID 20194902, Verbindung

Temperatur

90 °C

Dimethyl 6-methoxytetrahydropyran-3,3-dicarboxylate (6.6 g, 0.028 mol) was added to a solution of sodium hydroxide (2.8 g, 0.07 mol) in water (10 ml), and the mixture was heated at 90° C. for 3 hours. After the reaction mixture was cooled to 0° C., 6N hydrochloric acid (12 ml, 0.07 mol) was added to neutralize the solution. After salting out, the mixture was extracted with five 30 ml portions of ethyl ether. The combined ether extracts were dried over anhydrous magnesium sulfate, filtered, and subjected to rotary evaporation. The residual white powder was recystallized from a mixture of diethyl ether and acetone (3:1). Yield of the product, which decomposed at 136° to 140° C., was 94%.

1. temperatureAfter the reaction mixture was cooled to 0° C.
2. extractionthe mixture was extracted with five 30 ml portions of ethyl ether
3. dry with materialThe combined ether extracts were dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customsubjected to rotary evaporation
6. additionThe residual white powder was recystallized from a mixture of diethyl ether and acetone (3:1)
7. customdecomposed at 136° to 140° C.

ORD-Eintrag

ord-c6a894a420f34fe29a2761affca6e1a2

Quelldatensatz

uspto-grants-1987_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04677190