Acetic Acid → 1-Nitro-2-phenylethane

Temperatur

60 °C

Acetic acid (1.5 mL) was added to a solution of N,N-dibenzylethylene diamine (3.0 g, 12.5 mmol) in ethanol (25 mL) and the solution was stirred at 60° C. for 10 min A white solid formed which dissolved on heating to 80° C. Compound 3 (1.73 g, 6.25 mmol) was added and the stirring was continued at 80° C. for an additional 10 min. Paraformaldehyde (2.5. g, 88 mmol) was added to this solution in small portions over a period of 30 min and the suspension was stirred for 5 h at 80° C. Solvents were removed and the residue was treated with water. The pasty solid obtained was dissolved in ethyl acetate, washed with water and dried (Na2SO4). The oil obtained was purified by silica gel chromatography. (hexane/ethyl acetate, 9/1, 7/3). UV visible fractions were collected and evaporated to give 4 as an oil. Yield: 3.2 g (64%).

1. customformed which
2. dissolutiondissolved
3. temperatureon heating to 80° C
4. waitthe stirring was continued at 80° C. for an additional 10 min
5. stirringthe suspension was stirred for 5 h at 80° C
6. customSolvents were removed
7. additionthe residue was treated with water
8. customThe pasty solid obtained
9. washwashed with water
10. dry with materialdried (Na2SO4)
11. customThe oil obtained
12. customwas purified by silica gel chromatography
13. customUV visible fractions were collected
14. customevaporated

ORD-Eintrag

ord-610aa24dd232441789359085d983577f

Quelldatensatz

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08105567B2