Stannous Chloride → HCID 20450007, compound

HRID 358072Notes

Reaction equation

HRID 358072 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-])=O)[CH:17]=[CH:18][C:13]=2[N:12]2[C:22]([CH3:25])=[N:23][N:24]=[C:11]2[CH2:10][CH:9]=1.[Sn](Cl)Cl.C(=O)([O-])O.[Na+]>Cl>[NH2:19][C:16]1[CH:17]=[CH:18][C:13]2[N:12]3[C:22]([CH3:25])=[N:23][N:24]=[C:11]3[CH2:10][CH:9]=[C:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[C:14]=2[CH:15]=1

Participants

5

Reactant 3

HCID 24479Stannous ChlorideHCID 516892Sodium BicarbonateHCID 20450010HCID 20450010, compound

Product 1

HCID 20450007HCID 20450007, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A suspension of 195 mg of 6-(2-chlorophenyl)-1-methyl-8-nitro-4H-s-triazolo[4,3-a][1]benzazepine in 5 ml of concentrated hydrochloric acid is treated with 375 mg of tin (II) chloride, whereupon the mixture is heated to 50° for 40 hours while stirring. After cooling to room temperature, the mixture is neutralized with sodium hydrogen carbonate solution and extracted with chloroform. The chloroform extracts are dried and then evaporated. The residue is crystallized from ethyl acetate/ether, there being obtained 8-amino-6-(2-chlorophenyl)-1-methyl-4H-s-triazolo[4,3-a][1]benzazepine of melting point 271°-273°.

Workup

  1. temperatureis heated to 50° for 40 hours
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform extracts are dried
  4. customevaporated
  5. customThe residue is crystallized from ethyl acetate/ether, there

Sources & evidence

ORD record
ord-beda4460cddb485bb9fa986572a0af20
Source dataset
uspto-grants-1984_08
Patent number
US04464300

Reaction notes

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