2,5-Dichloro-4-nitroaniline → HCID 19431120, compound

HRID 1077377Notes

Reaction equation

HRID 1077377 reaction equation
[CH3:1][S-:2].[Na+].Cl[C:5]1[CH:10]=[C:9]([NH2:11])[C:8]([Cl:12])=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]>C(COC)OC.O>[CH3:1][S:2][C:5]1[CH:10]=[C:9]([NH2:11])[C:8]([Cl:12])=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]

Participants

5

Reactant 2

HCID 231082,5-Dichloro-4-nitroanilineHCID 4378561Sodium methanethiolate

Product 1

HCID 19431120HCID 19431120, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 80711,2-DimethoxyethaneSolvent

Procedure

To a suspension of 18.9 g (0.27 mol) of sodium thiomethoxide in 200 ml of dimethoxyethane, with stirring at room temperature, are added portionwise 41.4 g (0.2 mol) of 2,5-dichloro-4-aminonitrobenzene, allowing the temperature to rise to 50°-55° C. and maintaining this temperature for 1/2 hour after the addition is complete. The reaction medium is poured onto 2 liters of ice-water. The crystallized precipitate is drained, re-slurried in water and vacuum-dried at 40° C. over phosphorus pentoxide.

Workup

  1. customto rise to 50°-55° C.
  2. temperaturemaintaining this temperature for 1/2 hour
  3. additionafter the addition
  4. dry with materialvacuum-dried at 40° C. over phosphorus pentoxide

Sources & evidence

ORD record
ord-6e9563b913f54414bc4282e6cf390159
Source dataset
uspto-grants-1996_08
Patent number
US05542952

Reaction notes

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