Hydrochloric Acid → 3,4,5-Trifluorobenzyl alcohol

Then, 37.91 g of 3,4,5-trifluorobenzaldehyde and 10 mL of water were dissolved in 50 mL of ethanol and cooled with ice, and 2.69 g of sodium tetrahydroborate was slowly added to the resultant solution. The mixture was stirred at room temperature for 2 hours, and 10% hydrochloric acid was added until the system became acidic, followed by stirring for 1 hour. Then, hexane was added to the mixture to separate an organic layer, and an aqueous layer was subjected to extraction with hexane. The hexane extract was combined with the organic layer and washed with saturated brine. The resultant mixture was dried by adding sodium sulfate, and then the solvent was distilled off under reduced pressure. Then, reduced-pressure distillation (3.9 kPa, b. p.=116° C. to 118° C.) yielded 26.73 g of 3,4,5-trifluorobenzyl alcohol (A).

1. stirringby stirring for 1 hour
2. customto separate an organic layer
3. extractionan aqueous layer was subjected to extraction with hexane
4. extractionThe hexane extract
5. washwashed with saturated brine
6. dry with materialThe resultant mixture was dried
7. additionby adding sodium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. distillationThen, reduced-pressure distillation (3.9 kPa, b. p.=116° C. to 118° C.)

ORD record

ord-0e422af5bea64fa08cbbfa52e7751a76

Source dataset

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08916718B2