反应详情

A mixture containing 2-trifluoromethylphenyl isothiocyanate (0.82 g, 0.004 mol) and 6-(2-chlorophenyl)-7,8,9,10-tetrahydro-1-methyl-4H-pyrido[4′,3′;4,5]thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepine (1 g, 0.0027 mol) in 30 ml of 1,2-dichloroethane is agitated for 4 hours and at a temperature close to 20° C. Half the solvent is evaporated off with the rotary evaporator then 10 ml of ether is added. Agitation is carried out for 20 minutes at a temperature close to 20° C. followed by filtering on frit then washing with 20 ml of ether, with 20 ml of isopropyl ether and with 20 ml of isopentane. After drying under vacuum a cream coloured solid is obtained (1.21 g, 78%). Melting point: 190–192° C.

1. customclose to 20° C
2. customHalf the solvent is evaporated off with the rotary evaporator
3. addition10 ml of ether is added
4. waitAgitation is carried out for 20 minutes at a temperature
5. customclose to 20° C.
6. filtrationby filtering on frit
7. washthen washing with 20 ml of ether, with 20 ml of isopropyl ether and with 20 ml of isopentane
8. customAfter drying under vacuum a cream
9. customis obtained (1.21 g, 78%)