反应详情

210 mg (1.66 mmol) of oxalyl chloride are slowly added dropwise to a solution of 150 mg (0.28 mmol) of 4-{(3E)-4-{2-[(4-tert-butylbenzyl)oxy]phenyl}-2-[2-(4-cyanophenyl)ethyl]but-3-en-1-yl}benzoic acid from Example 105A in 1.5 ml of dry toluene with 2 drops of DMF while cooling in ice. The reaction mixture is stirred at RT for 5 minutes and then heated to reflux for 1 hour. After cooling, the mixture is concentrated in vacuo, and the residue is coevaporated twice with toluene and then taken up in 3 ml of THF. This solution is added to a previously prepared solution of 33.5 mg (0.30 mmol) of aminoguanidine hydrochloride and 22 mg (0.55 mmol) of sodium hydroxide in 1 ml of THF and 0.25 ml of water at 0° C. The mixture is stirred at 0° C. for 2 hours and then concentrated, and the residue is reacted without further purification in the next stage.

1. temperaturewhile cooling in ice
2. temperatureheated
3. temperatureto reflux for 1 hour
4. temperatureAfter cooling
5. concentrationthe mixture is concentrated in vacuo
6. stirringThe mixture is stirred at 0° C. for 2 hours
7. concentrationconcentrated
8. customthe residue is reacted without further purification in the next stage