Sulfuric Acid → HCID 40479468, compound
Reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]1[C:13]([F:14])=[CH:12][CH:11]=[C:10]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]=1C(OC)=O.S(=O)(=O)(O)O.[O:30]1CCC[CH2:31]1>>[F:7][C:8]1[CH:9]=[C:10]([C:15]2[CH:16]=[CH:17][C:18]([CH2:31][OH:30])=[CH:19][CH:20]=2)[CH:11]=[CH:12][C:13]=1[F:14]Participants
Conditions
- Temperature
- -10 °C
Procedure
Next, to a solution comprising 4 g of lithium aluminum hydride dissolved in 200 ml of tetrahydrofuran was added dropwise a solution comprising 30 g of the previously obtained methyl 3,4-difluorobiphenyl carboxylate and 100 ml of tetrahydrofuran with stirring at -10° C., and the mixture was stirred for one hour at the same temperature to proceed the reaction. After completion of the reaction, to the reaction mixture was added 30 g of sulfuric acid and the resulting mixture was extracted with toluene. The reaction mixture was washed with a saturated NaCl aqua, dried, and the solvent was removed under reduced pressure. The residue was purified by distillation under reduced pressure (165° C/1 mmHg) to obtain 28 g of 4-(3,4-difluorophenyl)benzyl alcohol.
Workup
- additionwas added dropwise a solution
- stirringthe mixture was stirred for one hour at the same temperature
- customthe reaction
- customAfter completion of the reaction
- extractionthe resulting mixture was extracted with toluene
- washThe reaction mixture was washed with a saturated NaCl aqua
- customdried
- customthe solvent was removed under reduced pressure
- distillationThe residue was purified by distillation under reduced pressure (165° C/1 mmHg)
Sources & evidence
- ORD record
- ord-bba3b87a011d4cd6aead5e9b56b91784
- Source dataset
- uspto-grants-1997_07
- Patent number
- US05651919
Reaction notes
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