Acetic Acid → HCID 14856511, compound

60 g (0.30 mols) of 3-bromoacetophenone are dissolved in 800 ml of ethanol and mixed with 250 ml of dimethylamine. The pH of the solution is adjusted to 6.5 with acetic acid. The reaction mixture is then cooled to 0° and mixed with 19 g of sodium cyanoborohydride. After stirring for 2 days at room temperature, the reaction mixture is concentrated. The residue is mixed with 800 ml of water and acidified. The solution is then extracted twice with 400 ml of ether, the aqueous phase is rendered basic and extraction follows 3× with 400 ml of ether. The combined organic extracts are dried and concentrated. After distillation of the residue, the 3-bromo-N,N,α-trimethylbenzenemethanamine is obtained; b.p.: 98°-100°/10 mmHg.

1. temperatureThe reaction mixture is then cooled to 0°
2. concentrationthe reaction mixture is concentrated
3. additionThe residue is mixed with 800 ml of water
4. extractionThe solution is then extracted twice with 400 ml of ether
5. extractionextraction
6. customThe combined organic extracts are dried
7. concentrationconcentrated
8. distillationAfter distillation of the residue

ORD record

ord-1b98835d83e349e6b02d379a92e11f20

Source dataset

uspto-grants-1992_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05166181