Oxalyl chloride → HCID 21054123, Verbindung

Temperatur

-20 °C

To a 500 mL round bottomed flask containing n-decylphosphonic acid diethyl ester, 22 g (79.0 mmol) was added to 100 mL of diethylether. This solution was stirred and cooled to −20° C. using an ice/salt water bath. Oxalyl Chloride (20.06 g, 158 mmol) was added in small portions over 45 minutes while maintaining the temperature at −20° C. The reaction mixture was then allowed to warm to room temperature and stirred for 24 hours. The solvent was removed by rotary evaporation to give a viscous liquid. The liquid was purified by vacuum distillation (boiling point: 126° C. at 0.4 mmHg) to give 15.5 g (73% yield) of the desired product. 1H NMR (400 MHz CDCl3): δ 4.2 (m, 2H), 2.0 (m, 2H), 1.6 (m, 2H), 1.2 (m, 17H), 0.75 (t, 3H).

1. temperaturewhile maintaining the temperature at −20° C
2. temperatureto warm to room temperature
3. stirringstirred for 24 hours
4. customThe solvent was removed by rotary evaporation
5. customto give a viscous liquid
6. distillationThe liquid was purified by vacuum distillation (boiling point: 126° C. at 0.4 mmHg)

ORD-Eintrag

ord-3f47dea63c0c44738ef2d9675961e690

Quelldatensatz

uspto-grants-2006_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07109184B2