Potassium bisulfate → HCID 54384020, compound

HRID 1756121Notes

Reaction equation

HRID 1756121 reaction equation
Cl.[CH2:2]([N:9]1[C:13]([CH:14](O)[CH2:15][CH2:16][CH:17]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:12][N:11]=[CH:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.S([O-])(O)(=O)=O.[K+]>C(O)C>[CH2:2]([N:9]1[C:13]([CH:14]=[CH:15][CH2:16][CH:17]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)=[CH:12][N:11]=[CH:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 516920Potassium bisulfateHCID 14822291HCID 14822291, compound

Product 1

HCID 54384020HCID 54384020, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1-benzyl-5-(1-hydroxy-4,4-diphenylbutyl)-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, 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 in methylene chloride, washed with water and evaporated to dryness. The product is then made to hydrochloride salt with dry hydrochloric acid in dry ethylacetate. Yield is 2,9 g. M.p. 204°-206° C.

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 in methylene chloride
  7. washwashed with water
  8. customevaporated to dryness

Sources & evidence

ORD record
ord-8ff3c1b1668a4c86852f8065368aaff3
Source dataset
uspto-grants-1995_08
Patent number
US05439928

Reaction notes

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