Hydrochloric Acid → HCID 21317683, compound

HRID 262984Notes

Reaction equation

HRID 262984 reaction equation
[C:1]([NH:4][NH:5][C:6]1[CH2:7][N:8]=[C:9]([C:17]2[C:22]([F:23])=[CH:21][CH:20]=[CH:19][C:18]=2[F:24])[C:10]2[CH:15]=[C:14]([Cl:16])[S:13][C:11]=2[N:12]=1)(=O)[CH3:2].Cl>C(Cl)Cl>[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[C:22]([F:23])=[CH:21][CH:20]=[CH:19][C:18]=3[F:24])[C:10]=2[CH:15]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21317684HCID 21317684, compound

Product 1

HCID 21317683HCID 21317683, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
270 °C

Procedure

0.35 g of 2-(2-acetylhydrazino)-7-chloro-5-(2,6-difluorophenyl)-3H-thieno[2,3-e]-1,4-diazepine are distributed on a metal plate in as thin as possible a layer and maintained at 270° C. for 1 minute in a sand bath. The melt is taken up in methylene chloride and shaken three times with 0.1-N hydrochloric acid in order to remove the starting material. The methylene chloride is distilled off and the product recrystallized from ethyl acetate containing active carbon. There is obtained 2-chloro-4-(2,6-difluorophenyl)-9-methyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine, melting point 185°-187° C.

Workup

  1. customto remove the starting material
  2. distillationThe methylene chloride is distilled off
  3. customthe product recrystallized from ethyl acetate containing active carbon

Sources & evidence

ORD record
ord-27fd9969174a4b17a98f518ea8be4d95
Source dataset
uspto-grants-1979_05
Patent number
US04155913

Reaction notes

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