반응 #350175

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7-chloro-5-(o-chlorophenyl)-1,3-dihydro-2H-thieno[2,3-e]-1,4-diazepine-2-thione

cyanoacetic acid hydrazide

→

2-chloro-4-(o-chlorophenyl)-9-cyanomethyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine

용매

methanol

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후처리

1. 1
   농축The solution is concentrated to 10 ml
2. 2
   workup.WAITleft
3. 3
   기타to crystallize
4. 4
   여과The 7-chloro-5-(o-chlorophenyl)-2-(2-cyanoacetylhydrazino)-3H-thieno[2,3-e]-1,4-diazepine, which is filtered off under a vacuum
5. 5
   기타dried
6. 6
   온도is refluxed for 2 hours in 150 ml of absolute xylene
7. 7
   기타The solution is evaporated
8. 8
   기타the residue recrystallized from ethyl acetate containing active carbon

실험 절차

1.2 g of 7-chloro-5-(o-chlorophenyl)-1,3-dihydro-2H-thieno[2,3-e]-1,4-diazepine-2-thione are refluxed for 1.5 hours together with 2 g of cyanoacetic acid hydrazide in 80 ml of absolute methanol, a dry nitrogen stream being conducted through the solution. The solution is concentrated to 10 ml and left to crystallize. The 7-chloro-5-(o-chlorophenyl)-2-(2-cyanoacetylhydrazino)-3H-thieno[2,3-e]-1,4-diazepine, which is filtered off under a vacuum and dried, is refluxed for 2 hours in 150 ml of absolute xylene. The solution is evaporated and the residue recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-chlorophenyl)-9-cyanomethyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine, melting point 217°-220° C.

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