Ammonia → HCID 19914159, compound

HRID 1090864Notes

Reaction equation

HRID 1090864 reaction equation
F[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].[NH3:14]>O1CCCC1>[F:8][C:6]1[C:5]([F:9])=[CH:4][C:3]([C:10]([F:13])([F:12])[F:11])=[C:2]([NH2:14])[CH:7]=1

Participants

4

Reactant 2

HCID 222Ammonia2×HCID 141302821,2,4-Trifluoro-5-(trifluoromethyl)benzene

Product 1

HCID 19914159HCID 19914159, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
140 °C

Procedure

225 g of 2,4,5-trifluorobenzotrifluoride in 600 ml of tetrahydrofuran were initially introduced into an autoclave and it was pressurized using 100 ml of liquid ammonia. The mixture was heated at 140° C. for 8 hours with stirring at 400 rpm and then cooled to 20° C. After releasing the pressure of the unused ammonia, the batch was distilled. 37 g of 4,5-difluoro-2-aminobenzotrifluoride were obtained in the forerun. The main amount distilled at 78° C./18 mbar and is, according to NMR spectroscopic findings, 2,5-difluoro-4-amino-benzotrifluoride (nD20 : 1.4560) having a yield of 154 g.

Workup

  1. temperaturecooled to 20° C
  2. distillationthe batch was distilled

Sources & evidence

ORD record
ord-f6f2257497624a0ca9e208aa66061fbb
Source dataset
uspto-grants-1992_01
Patent number
US05082971

Reaction notes

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