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Heptanedinitrile → 2-Aminocyclohex-1-ene-1-carbonitrile

HRID 62656
Notes
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Reaction equation

HRID 62656 reaction equation
[H-].[Na+].[C:3]([CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]#[N:11])#[N:4]>C1(C)C=CC=CC=1>[NH2:4][C:3]1[CH2:5][CH2:6][CH2:7][CH2:8][C:9]=1[C:10]#[N:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 12590HeptanedinitrileHCID 24758Sodium hydride

Product 1

HCID 2901752-Aminocyclohex-1-ene-1-carbonitrileYield 42.5%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

To cold toluene (20 mL) was added 60% NaH (720 mg, 18.0 mmol) slowly and followed by a solution of 1,5-dicyanopentane (2.1 mL, 16.37 mmol) in toluene (5 mL) slowly at 0° C. The resulting mixture was refluxed for 4 h and cooled to room temperature. The reaction mixture was quenched with ethanol (2 mL), water (20 mL) and acetic acid (2 mL). The organic layer was separated and aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure. Water was added to the crude residue, then filtered and washed with hexane to afford 850 mg (42%) of 2-aminocyclohex-1-enecarbonitrile (I-7a) as a pale brown solid.

Workup

  1. temperatureThe resulting mixture was refluxed for 4 h
  2. customThe reaction mixture was quenched with ethanol (2 mL), water (20 mL) and acetic acid (2 mL)
  3. customThe organic layer was separated
  4. extractionaqueous layer was extracted with ethyl acetate (3×20 mL)
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. additionWater was added to the crude residue
  9. filtrationfiltered
  10. washwashed with hexane

Sources & evidence

ORD record
ord-7166a091d9b64877a0ea22eb89e79094
Source dataset
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09447039B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes