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3-Hydroxybenzaldehyde → 3-(Oxiran-2-ylmethoxy)benzaldehyde

HRID 1051436
Notes
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Reaction equation

HRID 1051436 reaction equation
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[H-].[Na+].Cl[CH2:13][CH:14]1[CH2:16][O:15]1>CN(C=O)C>[O:15]1[CH2:16][CH:14]1[CH2:13][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 1013-HydroxybenzaldehydeHCID 7835EpichlorohydrinHCID 24758Sodium hydride

Product 1

HCID 27740493-(Oxiran-2-ylmethoxy)benzaldehydeYield 75%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent2×

Procedure

To a solution of 3-hydroxybenzaldehyde (2.0 g, 16.38 mmol) in DMF (25 mL) was added NaH (60%, 982.6 mg, 24.57 mmol) at 0° C. in portions. The mixture was stirred at this temperature for 30 minutes before a solution of 2-(chloromethyl)oxirane (2.27 g, 24.57 mmol) in DMF (5 mL) was slowly added into the reaction mixture which was then allowed to reach room temperature slowly and stirred for 16 h. The solvent was removed by concentration and the residue dissolved in ethyl acetate and washed with water. T the separated organic layer was dried over sodium sulfate, filtered and concentrated. The crude product was then purified by column chromatography. (2.2 g, yield 75%) MS (ESI+) e/z: 179.1 [M+1]+.

Workup

  1. additionwas slowly added into the reaction mixture which
  2. customto reach room temperature
  3. customThe solvent was removed by concentration
  4. dissolutionthe residue dissolved in ethyl acetate
  5. washwashed with water
  6. dry with materialT the separated organic layer was dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product was then purified by column chromatography

Sources & evidence

ORD record
ord-ceddf5b7c0eb47bfba1a72bdf3c9dd5e
Source dataset
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09388173B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes