Lithium borohydride → (4-Bromo-3-(trifluoromethoxy)phenyl)methanol

HRID 1749454Notes

Reaction equation

HRID 1749454 reaction equation
[BH4-].[Li+].[Br:3][C:4]1[CH:13]=[CH:12][C:7]([C:8](OC)=[O:9])=[CH:6][C:5]=1[O:14][C:15]([F:18])([F:17])[F:16]>C1COCC1>[Br:3][C:4]1[CH:13]=[CH:12][C:7]([CH2:8][OH:9])=[CH:6][C:5]=1[O:14][C:15]([F:16])([F:18])[F:17]

Participants

4

Conditions

Temperature
70 °C

Procedure

To a solution of lithium borohydride (1.16 g, 53.4 mmol) in THF (100 mL) was added methyl 4-bromo-3-(trifluoromethoxy)benzoate (10.6 g, 35.6 mmol) at 0° C., and the resulting solution was heated at 70° C. for 3 h under nitrogen atmosphere. The reaction was quenched with water and the mixture was extracted with ethyl acetate. The combined organic layers were washed with saturated brine, dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated under vacuum to afford the crude title product (9.17 g, 34 mmol). MS (ESI) m/z 270.1 M+, 272.1 [M+2]+.

Workup

  1. customThe reaction was quenched with water
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe combined organic layers were washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe filtrate was evaporated under vacuum

Sources & evidence

ORD record
ord-4038d9651be042f798ac1dea23501f5b
Source dataset
uspto-grants-2015_10
Patent number
US09156798B2

Reaction notes

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