Methyl 4-(2-bromoethyl)benzoate → [4-(2-Bromoethyl)phenyl]methanol

HRID 2360590Notes

Reaction equation

HRID 2360590 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Br:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](OC)=[O:17])=[CH:12][CH:11]=1>C1COCC1>[Br:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][OH:17])=[CH:12][CH:11]=1

Participants

4

Conditions

Temperature
0 °C

Procedure

To a suspension of LiAlH4 (4.5 mmol; 0.172 g) in anhydrous THF (5.0 ml) cooled to 0° C. was added dropwise a solution of methyl 4-(2-bromoethyl)benzenecarboxylate (1.0 g; 4.1 mmol) in anhydrous THF (10.0 ml). The reaction mixture was stirred for 5 minutes at room temperature and, after adding ice, was filtered through a Büchner filter. The solvent was removed under reduced pressure and the residue was extracted with ethyl acetate (3×100 ml). The combined organic phases were washed with saturated NaCl solution, dried over sodium sulfate and evaporated under reduced pressure. 800 mg (82.6%) of pure product were thus obtained as an oil.

Workup

  1. additionafter adding ice
  2. filtrationwas filtered through a Büchner
  3. filtrationfilter
  4. customThe solvent was removed under reduced pressure
  5. extractionthe residue was extracted with ethyl acetate (3×100 ml)
  6. washThe combined organic phases were washed with saturated NaCl solution
  7. dry with materialdried over sodium sulfate
  8. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-edc8e15a681a46709d415a097f36b4ae
Source dataset
uspto-grants-2014_04
Patent number
US08686147B2

Reaction notes

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