Trifluoroacetic acid → HCID 15023103, compound

HRID 1680956Notes

Reaction equation

HRID 1680956 reaction equation
[NH2:1][C:2]1[C:3]([NH:13][CH3:14])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[CH:9][C:8]([CH3:12])=[CH:7]2.[F:15][C:16]([F:21])([F:20])[C:17](O)=O.[OH-].[Na+]>Cl>[CH3:14][N:13]1[C:3]2[CH:4]=[CH:5][C:6]3[CH:7]=[C:8]([CH3:12])[CH:9]=[N:10][C:11]=3[C:2]=2[N:1]=[C:17]1[C:16]([F:21])([F:20])[F:15]

Participants

5

Reactant 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 15023102HCID 15023102, compound

Product 1

HCID 15023103HCID 15023103, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
95 °C

Procedure

A mixture of 5.61 g (30 mmol) of 8-amino-3-methyl-7-methylaminoquinoline and 3.02 ml (40 mmol) of trifluoroacetic acid in 40 ml of 4N hydrochloric acid is heated at 95° C. for 2 h. It is then allowed to cool to room temperature and poured into 250 g of ice, the pH is adjusted to 9 with concentrated sodium hydroxide solution, and the precipitate is filtered off with suction. The crude product is dried and recrystallized from ethyl acetate/petroleum ether.

Workup

  1. temperatureto cool to room temperature
  2. filtrationthe precipitate is filtered off with suction
  3. dry with materialThe crude product is dried
  4. customrecrystallized from ethyl acetate/petroleum ether

Sources & evidence

ORD record
ord-293af99076ad45138f5bcc2e4c17b151
Source dataset
uspto-grants-1992_12
Patent number
US05167695

Reaction notes

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