Hydrochloric Acid → HCID 10080858, compound

A suspension of (1S)-1-(2-methyl-2-propenoxymethyl)-3-methylbutylamine (51.9 g, 0.3 mol) and 5% Pd/C (10.4 g) in ethanol (520 mL) was stirred for 18 hours at room temperature in a hydrogen atmosphere (1 atm.). To the resulting reaction mixture was added 6 mol/L aqueous hydrochloric acid (52 mL) under cooling in ice bath. The aqueous mixture was subjected to filtration using celite for removing insolubles and then placed under reduced pressure for distilling the solvent off. The residue was dissolved in water, and the resulting aqueous solution was made to approx. pH 10 by addition of potassium carbonate. The solution was subjected to extraction with diethyl ether. The organic portion was dried over sodium sulfate and placed under reduced pressure for distilling off the solvent. There was obtained the titled compound (48.6 g, 92.6%) as an oily compound.

1. customTo the resulting reaction mixture
2. temperatureunder cooling in ice bath
3. filtrationThe aqueous mixture was subjected to filtration
4. customfor removing insolubles
5. distillationfor distilling the solvent off
6. dissolutionThe residue was dissolved in water
7. additionthe resulting aqueous solution was made to approx. pH 10 by addition of potassium carbonate
8. extractionThe solution was subjected to extraction with diethyl ether
9. dry with materialThe organic portion was dried over sodium sulfate
10. distillationfor distilling off the solvent

ORD record

ord-bb0a5667c66246d8989bbc8cec26495d

Source dataset

uspto-grants-2006_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07132573B2