HCID 21317679, compound → 6H-Thieno(3,2-f)(1,2,4)triazolo(4,3-a)(1,4)diazepine, 2-chloro-4-(2-chlorophenyl)-9-methyl-

HRID 262970Notes

Reaction equation

HRID 262970 reaction equation
[C:1]([NH:4][NH:5][C:6]1[CH2:7][N:8]=[C:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[C:10]2[CH:15]=[C:14]([Cl:16])[S:13][C:11]=2[N:12]=1)(=O)[CH3:2]>O>[Cl:16][C:14]1[S:13][C:11]2[N:12]3[C:1]([CH3:2])=[N:4][N:5]=[C:6]3[CH2:7][N:8]=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[Cl:23])[C:10]=2[CH:15]=1

Participants

3

Reactant 1

HCID 21317679HCID 21317679, compound

Product 1

HCID 30414556H-Thieno(3,2-f)(1,2,4)triazolo(4,3-a)(1,4)diazepine, 2-chloro-4-(2-chlorophenyl)-9-methyl-

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2.5 g of 2-(2-acetylhydrazino)-7-chloro-5-(o-chlorophenyl)-3H-thieno[2,3-e]-1,4-diazepine are heated under reduced pressure (water-jet vacuum) for 5-7 minutes in an oil bath (250° C.) until gas evolution is no longer observed. The resulting product is finely triturated in a mortar and boiled out several times with a total of 400 ml of ethyl acetate. After removal of the solvent, the resulting crude product is recrystallised from ethanol containing active carbon to give 2-chloro-4-(o-chlorophenyl)-9-methyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine in the form of cream-colored crystals, melting point 205°-206° C.

Workup

  1. customThe resulting product is finely triturated in a mortar
  2. customAfter removal of the solvent
  3. customthe resulting crude product is recrystallised from ethanol containing active carbon

Sources & evidence

ORD record
ord-326825d4c2b14d2f8fdaa2c099e2e8fa
Source dataset
uspto-grants-1979_05
Patent number
US04155913

Reaction notes

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