Hydrochloric Acid → HCID 23317128, compound

HRID 1982616Notes

Reaction equation

HRID 1982616 reaction equation
[OH-:1].[Na+].Cl[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][C:7]([N+:13]([O-:15])=[O:14])=[CH:6][C:5]=1[C:16]([F:19])([F:18])[F:17].Cl>>[F:17][C:16]([F:19])([F:18])[C:5]1[CH:6]=[C:7]([N+:13]([O-:15])=[O:14])[CH:8]=[C:9]([N+:10]([O-:12])=[O:11])[C:4]=1[OH:1]

Participants

4

Reactant 3

HCID 313Hydrochloric Acid2×HCID 14798Sodium HydroxideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-

Product 1

HCID 23317128HCID 23317128, compoundYield 90%

Conditions

Temperature
60 °C

Procedure

To a 1000 cm3 flask equipped with a stirrer, dropping funnel, reflux and thermometer 300 g /0.75 mole/ of a 10% by weight NaOH solution are added 81.3 g /0.3 mole/ of 2-chloro-3,5-dinitro-benzotrifluoride of a purity of 95% are added under stirring. The temperature is raised to 60° C. and the reaction mixture is stirred at 60°-65° C. for 4 hours, while the aqueous suspension forms an emulsion. The reaction mixture is then cooled to room temperature /20°-25° C./ under stirring and within 1 hour a 37% hydrochloric acid solution corresponding to 0.82 mole HCl is added in equal portions under vigorous stirring. The precipitated product is filtered, washed with water and dried to constant weight at room temperature. 2-Trifluoromethyl-4,6-dinitro-phenol is obtained /68.1 g., purity: 94%/ Idenfication was carried out by a mass spectrometer connected to a gas chromatograph.

Workup

  1. customTo a 1000 cm3 flask equipped with a stirrer
  2. temperaturereflux
  3. additionare added
  4. stirringthe reaction mixture is stirred at 60°-65° C. for 4 hours, while the aqueous suspension
  5. temperatureThe reaction mixture is then cooled to room temperature /20°-25° C./
  6. additionis added in equal portions under vigorous stirring
  7. filtrationThe precipitated product is filtered
  8. washwashed with water
  9. customdried to constant weight at room temperature

Sources & evidence

ORD record
ord-df08cb22551f4e17bf89c8646892ba31
Source dataset
uspto-grants-1986_06
Patent number
US04596893

Reaction notes

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