O-Phenylenediamine → 1,2-Benzenediamine,N1-(3-phenyl-2-propen-1-yl)-

3.24 g of ortho-phenylenediamine was dissolved in 30 ml of dimithylformaide, to the solution were added 2.07 g of potassium carbonate and 1.52 g of cinnamyl chloride, and the mixture was stirred overnight at a room temperature. After adding 100 ml of water, the reaction mixture was extracted twice with 100 ml and 50 ml of chloroform, and the extract was washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure The resulting residue was applied to a silica gel column and eluted with chloroform, to obtain 2.0 g of the title compound as light brown crystals.

1. extractionthe reaction mixture was extracted twice with 100 ml and 50 ml of chloroform
2. washthe extract was washed with a saturated sodium chloride aqueous solution
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customto remove the solvent under a reduced pressure The resulting residue
6. washeluted with chloroform

ORD-Eintrag

ord-fe25518ea9ed4d34b2044f4a465444f9

Quelldatensatz

uspto-grants-1993_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05245034