Methanol → HCID 20662437, compound

Temperature

0 °C

In a 50 ml flask, under a nitrogen atmosphere, 2-(2-fluoro-5-bromobenzyloxy)-(N,N-dimethyl)ethylamine (317 mg, 1.15 mmol) was dissolved in dichloroethane (3.5 ml). This solution was cooled to 0° C. and ACE•Cl (0.50 ml, 4.59 mmol) was added. The resulting mixture was warmed to ambient temperature, then heated to reflux and maintained at this temperature for about three hours. The progress of the reaction was monitored by thin layer chromatography. Methanol was added to the reaction mixture and the resulting mixture was stirred at ambient temperature for about three days. The mixture was then heated to reflux for thirty minutes. The solvents were removed in vacuo. The residue was taken up in methanol, heated to reflux for thirty minutes, and the solvents were then removed in vacuo. The title intermediate was used without further purification.

1. temperatureThe resulting mixture was warmed to ambient temperature
2. temperatureheated
3. temperatureto reflux
4. temperaturemaintained at this temperature for about three hours
5. temperatureThe mixture was then heated
6. temperatureto reflux for thirty minutes
7. customThe solvents were removed in vacuo
8. temperatureheated
9. temperatureto reflux for thirty minutes
10. customthe solvents were then removed in vacuo
11. customThe title intermediate was used without further purification

ORD record

ord-518014087f8d46e3a7ff94eff9100ce9

Source dataset

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06245761B1