HCID 23111595, compound → HCID 294499, compound

The obtained 5-benzhydrylamino-2-methylhexan-2-ol (5.20 g) was dissolved in methanol (250 ml), and thereafter, palladium hydroxide (2.00 g) was added to this solution. The mixture was then stirred in an autoclave under a hydrogen pressure of 9 kg/cm for 2.5 hours. The reaction solution was filtrated using a filter medium (Celite), and the filtrate was then concentrated under a reduced pressure. Thereafter, distilled water (50 ml) was added to the residue, and the liquid was then adjusted to be pH 2.0 by addition of 1 M hydrochloric acid. Thereafter, the solution was washed with diethyl ether (100 ml×3). The water layer was adjusted to be pH 12 by addition of an aqueous 6 M sodium hydroxide solution, followed by extraction with chloroform (100 ml×3). The organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The solvent was distilled off under a reduced pressure to obtain 5-amino-2-methyl-2-hexanol (2.01 g).

1. filtrationThe reaction solution was filtrated
2. concentrationthe filtrate was then concentrated under a reduced pressure
3. distillationThereafter, distilled water (50 ml)
4. additionwas added to the residue
5. additionby addition of 1 M hydrochloric acid
6. washThereafter, the solution was washed with diethyl ether (100 ml×3)
7. additionby addition of an aqueous 6 M sodium hydroxide solution
8. extractionfollowed by extraction with chloroform (100 ml×3)
9. washThe organic layer was washed with a saturated saline solution
10. dry with materialdried over anhydrous sodium sulfate
11. distillationThe solvent was distilled off under a reduced pressure

ORD record

ord-f91ff5a29566458cb58c573a6130d3c7

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07598244B2