Water → Triethylboroxine

HRID 1710208Notes

Reaction equation

HRID 1710208 reaction equation
C([B:3]([CH2:6][CH3:7])CC)C.[B]=O.[OH2:10]>>[CH2:6]([B:3]1[O:10][B:3]([CH2:6][CH3:7])[O:10][B:3]([CH2:6][CH3:7])[O:10]1)[CH3:7]

Participants

4

Reactant 3

HCID 962WaterHCID 7357TriethylboraneHCID 6327189Boron monoxide

Product 1

HCID 587242Triethylboroxine

Procedure

A 500 cc round bottom flask was equipped with water cooled reflux condenser an electrically heated mantle, and a nitrogen bubbler to maintain an inert atmosphere. To the flask under nitrogen was added 70.0 g of B2O3 (Aldrich Gold Label) which had been ground to a powder in a mortar under dry nitrogen. Neat triethylborane (100.0 g) was added to the boron oxide all at one time and the reaction flask was set up for refluxing. Reflux was continued for 5 days at which point the reflux condenser was changed for a distillation condenser and the liquid was distilled in two fractions. The second fraction yielded 60 cc of a colorless liquid which distilled at 148° C. The H-1 and B-11 NMR of the second fraction indicated that it was pure triethylboroxine.

Workup

  1. temperaturecooled
  2. temperaturereflux condenser an electrically heated mantle, and a nitrogen bubbler
  3. temperatureto maintain an inert atmosphere
  4. temperaturefor refluxing
  5. temperatureReflux
  6. customthe reflux condenser was changed for a distillation condenser
  7. distillationthe liquid was distilled in two fractions

Sources & evidence

ORD record
ord-d623febc45754a64896e1ab34694ce88
Source dataset
uspto-grants-1990_08
Patent number
US04952714

Reaction notes

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