反应详情

0.8 g of 7-chloro-5-(o-chlorophenyl)-1,3-dihydro-2H-thieno[2,3-e]-1,4-diazepine-2-thione are refluxed in 40 ml of absolute methanol with 1.5 g of oxalic acid amide hydrazide for 1.5 hours. The solution is concentrated to 10 ml and left to crystallize in a refrigerator. The filtered and dried 7-chloro-5-(o-chlorophenyl)-2-(2-oxalylamidohydrazino)-3H-thieno[2,3-e]-1,4-diazepine is refluxed in 100 ml of absolute xylene for 3 hours. The organic phase is evaporated and the residue recrystallized from ethanol to yield 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-carboxylic acid amide, melting point 248°-251° C.

1. concentrationThe solution is concentrated to 10 ml
2. waitleft
3. customto crystallize in a refrigerator
4. filtrationThe filtered
5. temperaturedried 7-chloro-5-(o-chlorophenyl)-2-(2-oxalylamidohydrazino)-3H-thieno[2,3-e]-1,4-diazepine is refluxed in 100 ml of absolute xylene for 3 hours
6. customThe organic phase is evaporated
7. customthe residue recrystallized from ethanol