Sulfuric Acid → HCID 20458453, compound

HRID 544637Notes

Reaction equation

HRID 544637 reaction equation
[NH2:1][C:2]1[CH2:6][CH:5]([CH3:7])[N:4]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:3]=1.[S:15](=[O:19])(=[O:18])([OH:17])[OH:16]>O>[S:15]([OH:19])([OH:18])(=[O:17])=[O:16].[NH2:1][C:2]1[CH2:6][CH:5]([CH3:7])[N:4]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:3]=1

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 15580678HCID 15580678, compound

Product 1

HCID 20458453HCID 20458453, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 4.0 g. of 3-amino-1-(p-fluorophenyl)-5-methyl-2-pyrazoline (prepared as described in Example 26), 25.0 ml. of water and 1.0 ml. of concentrated sulfuric acid is refluxed for 6 hours. The mixture is cooled and the precipitate is collected and the solid is recrystallized first from acetone-hexane, then from acetone to give 1.0 g. of the desired product as prisms, m.p. 164.5°-166.5° C.

Workup

  1. additionA mixture of 4.0 g
  2. temperatureThe mixture is cooled
  3. customthe precipitate is collected
  4. customthe solid is recrystallized first from acetone-hexane
  5. customfrom acetone to give 1.0 g

Sources & evidence

ORD record
ord-580a2e15d62641d5a8884800ebf5b883
Source dataset
uspto-grants-1984_05
Patent number
US04451479

Reaction notes

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