Isopropanol → HCID 131723675, compound

Participants

Reaction Conditions

Reaction Steps

23.88 g (0.04 mol) of the compound of Example 1 (as trifluoroacetic acid salt) were suspended in 400 ml of isopropanol. To this suspension was added at −15° C. under an inert gas atmosphere a previously prepared solution of thionyl chloride in isopropanol (for the preparation of this solution 10.4 ml of thionyl chloride had been added dropwise at −10 to −15° C. and unter an inert gas atmosphere within 5 min to 160 ml of isopropanol and the mixture had been stirred at −10° C. for further 20 min). After completion of the addition the temperature rose within 30 min to room temperature. Then, the meanwhile clear solution was heated at 60° C. under stirring for 7 hours. Stirring was continued without heating overnight. By TLC control, the reaction exhibited to be completed. Solvents were removed by rotary destination in vacuo. The residue was suspended in 100 ml of isopropanol and the isopropanol was removed in vacuo. The solid residue was triturated with diethylether and separated by suction filtration. The raw product was suspended in 120 ml of isopropanol, heated to reflux with 2.4 g of charcoal and filtered. After cooling, the colourless product was separated by filtration. Yield: 16.2 g of an off-white solid.

Provenance & Evidence