Potassium bisulfate → HCID 14723916, compound

HRID 330643Notes

Reaction equation

HRID 330643 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[C:19]([CH3:24])[CH:18]=2)(O)[CH2:9][C:10]2[N:14]([CH3:15])[N:13]=[N:12][N:11]=2)=[CH:4][C:3]=1[CH3:25].S([O-])(O)(=O)=O.[K+]>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[C:19]([CH3:24])[CH:18]=2)=[CH:9][C:10]2[N:14]([CH3:15])[N:13]=[N:12][N:11]=2)=[CH:4][C:3]=1[CH3:25]

Participants

4

Reactant 2

HCID 516920Potassium bisulfateHCID 14723915HCID 14723915, compound

Product 1

HCID 14723916HCID 14723916, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Conditions

Temperature
195 °C

Procedure

A mixture of 1,1-bis(4-fluoro-3-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol (3.58 g, 10.9 mmoles) and potassium hydrogen sulfate (530 mg) was heated at 195° C. for 1.5 hours. The mixture was cooled to 70° C. and chloroform (50 ml) was added. The insoluble material was removed by filtration and the filtrate evaporated. The residue was crystallized from EtOAc-Hexane to afford 3.38 g (100%) of the title compound; m.p.=138°-139° C.

Workup

  1. temperatureThe mixture was cooled to 70° C.
  2. customThe insoluble material was removed by filtration
  3. customthe filtrate evaporated
  4. customThe residue was crystallized from EtOAc-Hexane

Sources & evidence

ORD record
ord-64bcf8e94af44820b544230b2dd715d6
Source dataset
uspto-grants-1990_01
Patent number
US04897490

Reaction notes

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