3-Hydroxy-3-methylglutaric acid monoamide, ammonium salt → 3-Hydroxy-3-methylglutaric acid monoamide

1.79 g. (0.01 moles) of 3-hydroxy-3-methylglutaric acid monoamide, ammonium salt is dissolved in 50 ml of water and the solution is passed through a 100 ml column of Dowex 50 (H30 ) resin. The eluate is evaporated to dryness and the resulting residue dissolved in 100 ml of methanol containing 5 g. of hydrogen chloride. After 24 hours at room temperature the reaction mixture is evaporated to dryness under vacuum. The resulting residue is dissolved in 50 ml of water and the solution passed through a 50 ml column of Dowex 2 in the formate form. The column is eluted with 200 ml of water which is collected and evaporated under vacuum to afford 3-hydroxy-3-methylglutaric acid monoamide, methyl ester.

1. customThe eluate is evaporated to dryness
2. dissolutionthe resulting residue dissolved in 100 ml of methanol containing 5 g
3. customAfter 24 hours at room temperature the reaction mixture is evaporated to dryness under vacuum
4. dissolutionThe resulting residue is dissolved in 50 ml of water
5. washThe column is eluted with 200 ml of water which
6. customis collected
7. customevaporated under vacuum

ORD-Eintrag

ord-a1cace6f994a4cb09ba0a9a7ff45839e

Quelldatensatz

uspto-grants-1980_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04208204