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Hydrochloric Acid → (3S)-N-benzyl-3-amino-2-hydroxy-5-methylhexylamine dihydrochloride

HRID 1905331
Notes
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Reaction equation

HRID 1905331 reaction equation
[CH2:1]([NH:8][CH2:9][CH:10]([OH:27])[C@@H:11]([NH:16]C(OCC1C=CC=CC=1)=O)[CH2:12][CH:13]([CH3:15])[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:28]>CO.[Pd]>[ClH:28].[ClH:28].[CH2:1]([NH:8][CH2:9][CH:10]([OH:27])[C@@H:11]([NH2:16])[CH2:12][CH:13]([CH3:14])[CH3:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 56634722(3S)-N-benzyl-3-carbobenzoxyamino-2-hydroxy-5-methylhexylamine

Product 1

HCID 70395546(3S)-N-benzyl-3-amino-2-hydroxy-5-methylhexylamine dihydrochloride

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

To a solution of 100 mg of (3S)-3-carbobenzoxyamino-5-methyl-1,2-epoxyhexane in 10 ml of diethyl ether were added 2 g of dry silica gel and 0.1 ml of benzylamine, and the mixture was stirred for 16 hours at room temperature, then heated under reflux for 2 hours. After filtration of the silica gel, the filtrate was evaporated under reduced pressure. The residue was purified by preparative silica gel thin layer chromatography (developing solvent: lower layer of chloroform/methanol/water=8/3/1 by volume) to obtain 56 mg of (3S)-N-benzyl-3-carbobenzoxyamino-2-hydroxy-5-methylhexylamine as a colorless viscous oil. To a solution of 54 mg of the amine compound obtained in 10 ml methanol was added 0.2 ml of a 2N-hydrochloric acid. The mixture was hydrogenated over 10 mg of palladium charcoal under hydrogen atmosphere. After filtration of the catalyst, the filtrate was evaporated under reduced pressure to obtain 43 mg of (3S) -N-benzyl-3-amino-2-hydroxy-5-methylhexylamine dihydrochloride.

Workup

  1. filtrationAfter filtration of the catalyst
  2. customthe filtrate was evaporated under reduced pressure

Sources & evidence

ORD record
ord-dd3a7ddbf00e4e21a5be1f0ca4779e80
Source dataset
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04841067

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes