Formic Acid → HCID 64992220, compound

Temperature

80 °C

Into a mixture of 9.87 g of 4-bromobenzylamine hydrochloride and 5.04 g of triethylamine, 20 mL of a formic acid solution was dropped and the resultant reaction mixture was stirred at 80° C. for 3.5 hours. After the completion of the reaction, the reaction mixture was charged into 100 mL of ice water and the resultant reaction mixture was extracted with ethyl acetate (30 mL×2). The organic phase was dehydrated and dried over a saturated brine and anhydrous sodium sulfate in this order and the solvent was distilled off under reduced pressure. The residual solid was washed with hexane to obtain 9.29 g of the objective substance as a white crystal.

1. additionwas dropped
2. customthe resultant reaction mixture
3. customAfter the completion of the reaction
4. customthe resultant reaction mixture
5. extractionwas extracted with ethyl acetate (30 mL×2)
6. dry with materialdried over a saturated brine and anhydrous sodium sulfate in this order
7. distillationthe solvent was distilled off under reduced pressure
8. washThe residual solid was washed with hexane
9. customto obtain 9.29 g of the objective substance as a white crystal

ORD record

ord-5e22a5248a3249aea58fd384c137c161

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08268754B2