Tetrafluoroboric acid → HCID 20542103, compound

HRID 2286178Notes

Reaction equation

HRID 2286178 reaction equation
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:7]=[CH:8][C:9]2[N:15]([CH3:16])[C:14](=[O:17])[CH2:13][N:12]=[C:11]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[C:10]=2[CH:25]=1.[H+].[B-:27]([F:31])([F:30])([F:29])[F:28]>O>[F:28][B-:27]([F:31])([F:30])[F:29].[F:24][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[C:11]1[C:10]2[CH:25]=[C:6]([N+:5]#[N:1])[CH:7]=[CH:8][C:9]=2[N:15]([CH3:16])[C:14](=[O:17])[CH2:13][N:12]=1

Participants

5

Reactant 3

HCID 28118Tetrafluoroboric acidHCID 922947-AminoflunitrazepamHCID 23668193Sodium Nitrite2×

Product 1

HCID 20542103HCID 20542103, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

A solution of 2.9 g (42 mmol) of sodium nitrite in 7 ml of water is added while stirring to a solution, cooled in ice, of 11 g (38.8 mmol) of 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one in 50 ml of water and 100 ml of 50 percent aqueous hydrofluoboric acid so that the sodium nitrite solution enters below the surface of the mixture (addition time ca 15 minutes). The mixture is stirred at 5° for a further 30 minutes and then left to stand at -24° for 22 hours. The precipitated crystals are filtered off, washed with isopropanol and ether and dried at 14 Torr and room temperature. There is obtained 5-(o-fluorophenyl)-2,3-dihydro-1-methyl-2-oxo-1H-1,4-benzodiazepine-7-diazonium tetrafluoroborate (1:2) of melting point 120°-125°.

Workup

  1. additionenters below the surface of the mixture (addition time ca 15 minutes)
  2. stirringThe mixture is stirred at 5° for a further 30 minutes
  3. waitleft
  4. filtrationThe precipitated crystals are filtered off
  5. washwashed with isopropanol and ether
  6. customdried at 14 Torr and room temperature

Sources & evidence

ORD record
ord-7e84f70d249246b088838a1533056b7d
Source dataset
uspto-grants-1982_04
Patent number
US04327026

Reaction notes

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