Hydrochloric Acid → ST51022620

HRID 620916Notes

Reaction equation

HRID 620916 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][NH2:11].[C:12](OCC)(=[O:17])[CH2:13][C:14]([CH3:16])=O.[OH-].[K+].Cl>C(O)C.O>[CH3:16][C:14]1[CH2:13][C:12](=[O:17])[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=2[Cl:9])[N:11]=1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 8868Ethyl AcetoacetateHCID 14797Potassium HydroxideHCID 79234(2,4,6-Trichlorophenyl)hydrazine

Product 1

HCID 2825130ST51022620

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

To 280 g of 2,4,6-trichlorophenylhydrazine was added 180 ml of ethyl acetoacetate, and the resulting mixture was stirred at room temperature for 30 minutes. After adding thereto a solution prepared by dissolving 215 g of potassium hydroxide in 7 l of ethanol, the reaction solution was refluxed with heating for 1 hour. The reaction solution was poured into 6 l of water and neutralized with conc. hydrochloric acid. After being cooled to room temperature, a precipitate thus formed was filtered off, washed with water, and then dried under reduced pressure to obtain the titled compound. Yield: 300 g. Melting point: 178° to 180° C.

Workup

  1. additionAfter adding
  2. customa solution prepared
  3. temperaturethe reaction solution was refluxed
  4. temperaturewith heating for 1 hour
  5. temperatureAfter being cooled to room temperature
  6. customa precipitate thus formed
  7. filtrationwas filtered off
  8. washwashed with water
  9. customdried under reduced pressure

Sources & evidence

ORD record
ord-a1eb88bdba4247e68f3b14686c7d0efb
Source dataset
uspto-grants-1989_04
Patent number
US04822891

Reaction notes

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