Bromide ion → Benzo[b]quinolizinium hexafluorophosphate

HRID 742441Notes

Reaction equation

HRID 742441 reaction equation
[Br-].[CH:2]1[C:11]2[CH:10]=[C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]3=[CH:7][N+:6]=2[CH:5]=[CH:4][CH:3]=1.[F:16][P-:17]([F:22])([F:21])([F:20])([F:19])[F:18].[K+].[Br-]>O>[F:16][P-:17]([F:22])([F:21])([F:20])([F:19])[F:18].[CH:2]1[C:11]2[CH:10]=[C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]3=[CH:7][N+:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 259Bromide ionHCID 202130Benzo(b)quinolizinium, bromide (1:1)HCID 23688904Potassium hexafluorophosphate

Product 1

HCID 15186209Benzo[b]quinolizinium hexafluorophosphateYield 94.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

Benzo[b]quinolizinium bromide (508.5 g, 1.95 mol) was dissolved in 5 L of distilled water with heating (steam-bath). Potassium hexafluorophosphate (367.2 g, 1.95 mol) was dissolved in 1.1 L of water with heating and the resulting solution was poured in portions into the above bromide solution with steam-bath heating (20 min). The precipitate was formed immediately and the mixture was stirred at room temperature for 3 h, then stirred 1 h in an ice-water bath. The solid was filtered, washed with cold water (800 mL), dried (50°-60° C.) in vacuo for 3 days to afford 601 g (94.8%) of benzo[b]quinolizinium hexafluorophosphate. (Formula lI: R1 =R2 =R7 =H; X- --=PF6-).

Workup

  1. temperaturewith heating (steam-bath)
  2. temperaturewith heating
  3. temperatureheating (20 min)
  4. customThe precipitate was formed immediately
  5. stirringstirred 1 h in an ice-water bath
  6. filtrationThe solid was filtered
  7. washwashed with cold water (800 mL)
  8. customdried (50°-60° C.) in vacuo for 3 days

Sources & evidence

ORD record
ord-2cdff59ae1c44c3abae0908a3b242acb
Source dataset
uspto-grants-1996_09
Patent number
US05554620

Reaction notes

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