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Triethylamine → m-Phenoxybenzyl cyanide

HRID 584352
Notes
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Reaction equation

HRID 584352 reaction equation
[O:1]([C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=1)[CH2:11]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]([N:18](CC)CC)C>C(OCC)(=O)C.CS(Cl)(=O)=O>[O:1]([C:8]1[CH:9]=[C:10]([CH2:11][C:16]#[N:18])[CH:13]=[CH:14][CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 8471TriethylamineHCID 262953-Phenoxybenzyl alcohol

Product 1

HCID 40075m-Phenoxybenzyl cyanideYield 32%

Reagents, catalysts & solvents 2

HCID 8857Ethyl AcetateSolventHCID 31297Methanesulfonyl chlorideSolvent

Procedure

To a solution of 3-phenoxybenzylalcohol (25.0 g) and triethylamine (26.3 ml) in ethyl acetate (300 ml), methanesulfonyl chloride (14.6 ml) was added dropwise at 0° C. After stirring for 1 hour, the reaction mixture was washed with saturated aqueous sodium chloride, dried (MgSO4) and concentrated. The residue was dissolved in acetone (300 ml), admixed with sodium iodide (37.5 g) and then stirred for 1 hour. The reaction mixture was concentrated, and the residue was diluted with water and then extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and then concentrated. The residue was dissolved in dimethyl sulfoxide (100 ml) and stirred with sodium cyanide (7.35 g) for 15 hours at room temperature. The reaction mixture was diluted with ethyl acetate, washed with water, dried (MgSO4), and then concentrated. The residue was subjected to column chromatography on silica gel to obtain 3-phenoxyphenylacetonitrile (8.36 g, yield 32%) as an oil from a fraction eluted with ethyl acetate-hexane (1:7. v/v).

Workup

  1. washthe reaction mixture was washed with saturated aqueous sodium chloride
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in acetone (300 ml)
  5. stirringstirred for 1 hour
  6. concentrationThe reaction mixture was concentrated
  7. additionthe residue was diluted with water
  8. extractionextracted with ethyl acetate
  9. washThe ethyl acetate layer was washed with water
  10. dry with materialdried (MgSO4)
  11. concentrationconcentrated
  12. dissolutionThe residue was dissolved in dimethyl sulfoxide (100 ml)
  13. stirringstirred with sodium cyanide (7.35 g) for 15 hours at room temperature
  14. additionThe reaction mixture was diluted with ethyl acetate
  15. washwashed with water
  16. dry with materialdried (MgSO4)
  17. concentrationconcentrated

Sources & evidence

ORD record
ord-641bab9e2a0943d386ef1cd4bfeb9dbd
Source dataset
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06924300B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes