反应详情

A suspension of 194 mg 2-Cyano-5-methyl-3H-imidazole-4-carboxylic acid ethyl ester, 301 mg 3-Bromomethyl-5-(5-chloro-thiophen-2-yl)-isoxazole and 150 mg K2CO3 in 2 ml DMF was stirred for 5 h at RT. After addition of 2 ml brine the mixture was filtered through a chem elut® cartridge by elution with ethyl acetate and then concentrated under reduced pressure. The residue was then dissolved in 5 ml THF/MeOH/water 3:1:1 and treated with 30 mg LiOH monohydrate at RT. Then the solvent was removed under reduced pressure and the residue was taken-up in 5 ml 5 M HCl. The acid precipitated as a brown solid and was dried under reduced pressure. Yield: 280 mg

1. filtrationwas filtered through a chem elut® cartridge by elution with ethyl acetate
2. concentrationconcentrated under reduced pressure
3. dissolutionThe residue was then dissolved in 5 ml THF/MeOH/water 3:1:1
4. additiontreated with 30 mg LiOH monohydrate at RT
5. customThen the solvent was removed under reduced pressure
6. customThe acid precipitated as a brown solid
7. customwas dried under reduced pressure