Acetic Acid → HCID 23022395, compound

Temperature

80 °C

Triethylamine (1.52 g), N-(3-aminophenyl)acetamide (0.50 g) and n-butanol (2 mL) were added to a suspension of 3-(dimethylimino)-2-[(dimethylimino)methyl]-N,N-dimethyl-1-propene-1-aminium trichloride (1.45 g) in n-butanol (8 mL) at room temperature and were dissolved therein. The resulting solution was heated to 80° C., stirred for 3 hours and then cooled to room temperature. After addition of water (1 mL) to the reaction mixture, the solvent was distilled off under reduced pressure. The residue thus obtained was dissolved by addition of acetic acid (2 mL) and water (10 mL) and, again, the solvent was distilled off under reduced pressure. The resulting residue was dissolved by addition of water (10 mL) and the solution was adjusted to pH 8 with sodium hydrogen carbonate. After stirred at room temperature for 1 hour, precipitated crystals were collected by filtration and washed with water (10 mL). The crystals were dried under reduced pressure to obtain the title compound (0.63 g) as pale yellow crystals. Yield: 89%.

1. dissolutionwere dissolved
2. temperaturecooled to room temperature
3. distillationthe solvent was distilled off under reduced pressure
4. customThe residue thus obtained
5. distillationagain, the solvent was distilled off under reduced pressure
6. dissolutionThe resulting residue was dissolved by addition of water (10 mL)
7. stirringAfter stirred at room temperature for 1 hour
8. customprecipitated crystals
9. filtrationwere collected by filtration
10. washwashed with water (10 mL)
11. customThe crystals were dried under reduced pressure

ORD record

ord-f9aa9354e599419e939cfdde185cb9dd

Source dataset

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08373007B2