Phosphoric Acid → 2-Bromo-N,N-dibutylacetamide

Temperatur

0 °C

To a solution of bromoacetyl bromide (72.3 mL, 830 mmol) in toluene (500 mL) cooled to 0° C. was added a solution of dibutylamine (280.0 mL, 1.66 mol) in toluene (220 mL) via an addition funnel maintaining the reaction temperature below 10° C. Upon completion of the addition, the reaction mixture was stirred at 0° C. for 15 minutes. A solution of 2.5% aqueous H3PO4 (500 mL) was slowly introduced, and the reaction mixture was allowed to warm to room temperature with vigorous stirring. The solution is 2.5% phosphoric acid by weight. The layers were separated and the organic phase washed with water (500 mL) and concentrated to provide the bromoacetamide as a solution in toluene.

1. temperaturemaintaining the reaction temperature below 10° C
2. additionUpon completion of the addition
3. temperatureto warm to room temperature with vigorous stirring
4. customThe layers were separated
5. washthe organic phase washed with water (500 mL)
6. concentrationconcentrated

ORD-Eintrag

ord-15ecc8365a40437387ebf6c1b331eeec

Quelldatensatz

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06946481B1