Potassium bisulfate → HCID 14539528, compound

HRID 974478Notes

Reaction equation

HRID 974478 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])=[CH:19][CH:18]=2)(O)[CH2:9][C:10]2[N:14]([CH3:15])[N:13]=[N:12][N:11]=2)=[CH:4][CH:3]=1.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:18]=[CH:19][C:20]([F:23])=[CH:21][CH:22]=2)=[CH:9][C:10]2[N:14]([CH3:15])[N:13]=[N:12][N:11]=2)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 516920Potassium bisulfateHCID 14723979HCID 14723979, compound

Product 1

HCID 14539528HCID 14539528, compoundYield 102.9%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Conditions

Temperature
195 °C

Procedure

A mixture of 1,1-bis(4-fluorophenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol(4.2 g, 12.7 mmoles) [prepared in Step A] and potassium hydrogen sulfate was heated at 195° C. for 0.5 hour. After cooling, the mixture was dissolved in chloroform and washed with water. The organic layer was dried and evaporated in vacuo. The residue was triturated with diethyl ether to give 3.9 g of the title compound; m.p.=169°-171° C.

Workup

  1. temperatureAfter cooling
  2. washwashed with water
  3. customThe organic layer was dried
  4. customevaporated in vacuo
  5. customThe residue was triturated with diethyl ether

Sources & evidence

ORD record
ord-4edec8c87bd74cd28888b9e2dfb23521
Source dataset
uspto-grants-1991_11
Patent number
US05068346

Reaction notes

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