Tetrafluoroboric acid → HCID 22754124, compound

HRID 2163155Notes

Reaction equation

HRID 2163155 reaction equation
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[CH:5][C:6]([CH3:10])=[C:7]([CH:9]=1)[NH2:8].[H+].[B-:14]([F:18])([F:17])([F:16])[F:15].[N:19]([O-])=O.[Na+]>O>[F:15][B-:14]([F:18])([F:17])[F:16].[F:1][C:2]([F:11])([F:12])[C:3]1[CH:4]=[CH:5][C:6]([CH3:10])=[C:7]([N+:8]#[N:19])[CH:9]=1

Participants

5

Reactant 3

HCID 28118Tetrafluoroboric acidHCID 27359332-Methyl-5-(trifluoromethyl)anilineHCID 23668193Sodium Nitrite

Product 1

HCID 22754124HCID 22754124, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Seventeen and one-half grams of 5-trifluoromethyl-2-methylaniline was melted and the melted material added to 100 ml. of a cold 48 percent HBF4 solution. 7.9 g. of sodium nitrite in 10 ml. of water were added thereto in dropwise fashion. The temperature of the diazotization reaction was maintained below 15° C. during the addition. The diazotization mixture was stirred in the cold for about 15 minutes and then poured onto a sintered glass funnel. 5-Trifluoromethyl-2-methylphenyldiazonium fluorborate formed in the above reaction was collected thereon as a solid precipitate. The filter cake was washed once with cold HBF4 solution, twice with cold ethanol and several times with cold ether; weight = 20.2 g.; m.p. above 250° C.

Workup

  1. additionthe melted material added to 100 ml
  2. customThe temperature of the diazotization reaction
  3. temperaturewas maintained below 15° C. during the addition
  4. additionpoured onto a sintered glass funnel

Sources & evidence

ORD record
ord-b323e88b988347a49b2374b7fcfd8b6d
Source dataset
uspto-grants-1979_01
Patent number
US04132737

Reaction notes

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