Potassium bisulfate → HCID 178505675, compound

HRID 1756135Notes

Reaction equation

HRID 1756135 reaction equation
Cl.[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:21]2[N:22]=[CH:23][NH:24][CH:25]=2)(O)[CH2:10][CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:5][CH:4]=1.S([O-])(O)(=O)=O.[K+]>C(O)C>[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:21]2[N:22]=[CH:23][NH:24][CH:25]=2)=[CH:10][CH2:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:5][CH:4]=1

Participants

4

Reactant 2

HCID 516920Potassium bisulfateHCID 178479687HCID 178479687, compound

Product 1

HCID 178505675HCID 178505675, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

4-[1-(4-fluorophenyl)-1-hydroxy-5-phenylpentyl]-1H-imidazole hydrochloride (5,0 g) and 30,0 g of anhydrous potassium hydrogen sulphate are heated at 150° C. for 4 hours. The mixture is cooled and 90 ml of ethanol is added to dissolve the product. The mixture is then filtered and the filtrate is evaporated to minor volume. Water is added and the mixture is made alkaline with sodium hydroxide. The product is extracted into methylene chloride, washed with water and evaporated to dryness. The product is then made to hydrochloride salt with dry hydrogen chloride in dry ethylacetate.

Workup

  1. temperatureThe mixture is cooled
  2. dissolutionto dissolve the product
  3. filtrationThe mixture is then filtered
  4. customthe filtrate is evaporated to minor volume
  5. additionWater is added
  6. extractionThe product is extracted into methylene chloride
  7. washwashed with water
  8. customevaporated to dryness

Sources & evidence

ORD record
ord-f1ff40d895084115b005a2287f71007c
Source dataset
uspto-grants-1995_08
Patent number
US05439928

Reaction notes

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