Ammonium Hydroxide → HCID 13055817, compound

HRID 443575Notes

Reaction equation

HRID 443575 reaction equation
[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11]3=[N:18][NH:19][N:20]=[C:10]3[CH2:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N+:21]([O-])([O-:23])=[O:22].[K+].[OH-].[NH4+]>S(=O)(=O)(O)O>[N+:21]([C:5]1[CH:6]=[C:1]([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[C:11]3=[N:18][NH:19][N:20]=[C:10]3[CH2:9][N:8]=2)[CH:2]=[CH:3][CH:4]=1)([O-:23])=[O:22]

Participants

5

Reactant 3

HCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 30604501,2,3-Triazolo(4,5-d)(2)benzazepine, 2,4-dihydro-6-phenyl-

Product 1

HCID 13055817HCID 13055817, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Conditions

Temperature
0 °C

Procedure

A mixture of 1.6 g (4.5 mmole) of the methanesulfonate salt of 6-phenyl-2H,4H-[1,2,3]triazolo[4,5-d][2]benzazepine, 8.6 g of potassium nitrate, and 20 ml of sulfuric acid was stirred at 0° C. for 3.5 hr. The mixture was poured over ice, basified with ammonium hydroxide and extracted with methylene chloride. The methylene chloride solution was dried with anhydrous sodium sulfate and concentrated at reduced pressure. The residue was triturated with ether to give tan crystals (mp 223°-225° C.). Recrystallization from methylene chloride gave cream colored prisms, mp 224°-225° C.

Workup

  1. additionThe mixture was poured over ice
  2. extractionextracted with methylene chloride
  3. dry with materialThe methylene chloride solution was dried with anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure
  5. customThe residue was triturated with ether

Sources & evidence

ORD record
ord-b2dba3b8336f45cf9a061b908009972d
Source dataset
uspto-grants-1981_04
Patent number
US04260772

Reaction notes

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