Reaktion #1858630

Reaktionsgleichung

Iodomethane

NaH

methyl 1,3-dihydrobenzo[de]isochromene-1-carboxylate

DMF

EtOAc DCM triethyl amine

→

title compound

2-(1-Methyl-1,3-dihydrobenzo[de]isochromen-1-yl)-4,5-dihydro-1H-imidazole

Lösungsmittel

THF

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at ambient temperature for 3 hrs
2. 2
   SonstigeThe intermediate methyl 1-methyl-1,3-dihydrobenzo[de]isochromene-1-carboxylate (0.3 g) was purified with separation method A and E (EtOAc/heptanes)

Vorschrift

The mixture of NaH (0.18 g), methyl 1,3-dihydrobenzo[de]isochromene-1-carboxylate (0.5 g) and DMF (2 ml), toluene (2 ml) and THF (6 ml) was stirred in ice-bath temperature. Iodomethane (0.7 ml) was added and the mixture was stirred at ambient temperature for 3 hrs. The intermediate methyl 1-methyl-1,3-dihydrobenzo[de]isochromene-1-carboxylate (0.3 g) was purified with separation method A and E (EtOAc/heptanes), and the title compound was synthesized using the procedure of synthesis method A step 3 and separation method E (EtOAc/DCM/triethyl amine 10/20/1). (Yield 0.1 g).

Quelle