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2-(Adamantan-1-yl)ethan-1-amine hydrochloride → 1-C-Ethylaminoadamantane

HRID 1725856
Notes
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Reaction equation

HRID 1725856 reaction equation
Cl.[C:2]12([CH2:12][CH2:13][NH2:14])[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[CH2:3]1)[CH2:9]2>C(Cl)(Cl)Cl>[C:2]12([CH2:12][CH2:13][NH2:14])[CH2:9][CH:8]3[CH2:7][CH:6]([CH2:5][CH:4]([CH2:10]3)[CH2:3]1)[CH2:11]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 27711382-(Adamantan-1-yl)ethan-1-amine hydrochloride

Product 1

HCID 642451-C-Ethylaminoadamantane

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

Next, 2-(1-adamantyl)ethylamine hydrochloride (2.0 g, 9.3 mmol) was distributed with chloroform (30 ml) and a 1 N aqueous sodium hydroxide solution (40 ml), and the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 2-(1-adamantyl)ethylamine. Methanol (15 ml) and triethylamine (2.6 ml, 19 mmol) were added to 2-(1-adamantyl)ethylamine, and the mixture was stirred at room temperature. Then, a solution of 2-butynal (0.80 g, 12 mmol) obtained by the above-mentioned reaction in methanol (10 ml) was added to the mixture, and after three hours, sodium borohydride (1.9 g, 50 mmol) was added thereto under ice-cold water-cooling. After one hour, water (40 ml) was added to the reaction mixture, and the whole was extracted with chloroform (60 ml). The organic layer was washed with saturated brine (40 ml) and dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give 0.48 g (22%) of the titled compound as a brown oily matter.

Workup

  1. dry with materiala 1 N aqueous sodium hydroxide solution (40 ml), and the organic layer was dried over anhydrous magnesium sulfate
  2. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-8f08365bd24b412a82f677c4e200d5ab
Source dataset
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07491739B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes