HCID 178486879, compound → HCID 178486845, compound

Participants

Reaction Conditions

Reaction Steps

210 g of 3,4-dihydro-4-oxo-6-[trans-4-(4-methyl-3-oxo-piperazin-1-yl)-cyclohexyloxy]-7-methoxy-quinazoline hydrochloride [(V) HCl] in 1680 ml acetonitrile are refluxed and 840 ml of solvent are distilled off (elimination of traces of water). 221.4 g triphenylphosphine in 840 ml dioxane are added. 119.4 g of N-chlorosuccinimide in 600 ml acetonitrile are added. 260 ml acetonitrile are added. The mixture is stirred for 45 min at 80° C. and then cooled to 30° C. 8.94 ml of water and 420 ml dioxane are added. The precipitate is filtered off under protective gas and washed with 1200 ml THF. The product is precipitated as the hydrochloride and is processed further without drying. A small amount was dried and the yield can be calculated as approx. 210 g in relation thereto.

Provenance & Evidence