反应详情

A mixture containing 2-trifluoromethylbenzylisothiocyanate (1 g, 0.0046 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 (1.22 g, 0.0033 mol) in 20 ml of dichloromethane is agitated at a temperature close to 20° C. for 1 hour. The reaction mixture is evaporated to dryness. 40 ml of ethyl acetate is added to the residual oil. After separation of the insoluble part, the solvent is evaporated off. 40 ml of isopropyl ether is added until precipitation of the product then filtration on frit and washing with isopropyl ether. The solid obtained (1.2 g, 63%) is dried and a beige powder is obtained. Melting point: 178–184° C.

1. customclose to 20° C. for 1 hour
2. customThe reaction mixture is evaporated to dryness
3. addition40 ml of ethyl acetate is added to the residual oil
4. customAfter separation of the insoluble part
5. customthe solvent is evaporated off
6. addition40 ml of isopropyl ether is added until precipitation of the product
7. filtrationfiltration on frit
8. washwashing with isopropyl ether
9. customThe solid obtained (1.2 g, 63%)
10. customis dried
11. customa beige powder is obtained