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Hydrochloric Acid → (4-Tert-butyl-benzyl)-[2-(3-fluoro-5-trifluoromethyl-phenyl)-ethyl]-amine

HRID 855219
Notes
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Reaction equation

HRID 855219 reaction equation
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.[F:14][C:15]1[CH:16]=[C:17]([CH2:25][CH2:26][NH2:27])[CH:18]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:20]=1.C(=O)([O-])[O-].[K+].[K+].[BH4-].[Na+].Cl>CO>[C:1]([C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH:27][CH2:26][CH2:25][C:17]2[CH:18]=[C:19]([C:21]([F:22])([F:23])[F:24])[CH:20]=[C:15]([F:14])[CH:16]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 703244-tert-ButylbenzaldehydeHCID 4311764Sodium borohydrideHCID 685635402-(3-Fluoro-5-trifluoromethyl-phenyl)-ethylamine hydrochloride

Product 1

HCID 58568402
(4-Tert-butyl-benzyl)-[2-(3-fluoro-5-trifluoromethyl-phenyl)-ethyl]-amine
Yield 90%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3.1 ml of 4-tert-butylbenzaldehyde (18.47 mmol), 3 g of 2-(3-fluoro-5-trifluoromethyl -phenyl)-ethylamine hydrochloride (12.3 mmol) and 1.7 g of potassium carbonate (12.3 mmol) were suspended in 36 ml methanol at rt, and after stirring for 30 min at rt, were refluxed for 2 h. After cooling down to rt, 700 mg (18.47 mmol) of sodium borohydride were added and after stirring for 5 min at rt, the reaction mixture was refluxed for 2.5 h. After cooling down to rt, the reaction mixture was treated with 2.4 ml 1 N HCl and concentrated in vacuo. The residue was diluted with water/EtOAc. After separation of the organic phase, the aqueous phase was extracted with EtOAc and the combined organic phases were washed with brine, dried with magnesium sulfate, filtered off and concentrated in vacuo. The residue was purified by column chromatography (90 g silica gel; EtOAc/heptane 1:2) to give 4.35 g light yellow oil (90%). MS (ISP) 354.3 (M+H)+.

Workup

  1. temperaturewere refluxed for 2 h
  2. temperatureAfter cooling down to rt
  3. stirringafter stirring for 5 min at rt
  4. temperaturethe reaction mixture was refluxed for 2.5 h
  5. temperatureAfter cooling down to rt
  6. concentrationconcentrated in vacuo
  7. additionThe residue was diluted with water/EtOAc
  8. customAfter separation of the organic phase
  9. extractionthe aqueous phase was extracted with EtOAc
  10. washthe combined organic phases were washed with brine
  11. dry with materialdried with magnesium sulfate
  12. filtrationfiltered off
  13. concentrationconcentrated in vacuo
  14. customThe residue was purified by column chromatography (90 g silica gel; EtOAc/heptane 1:2)

Sources & evidence

ORD record
ord-c94a5120d5c34852a7ecfd2a07b5a0c5
Source dataset
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07259183B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes