Potassium Acetate → HCID 178526764, compound

HRID 1672315Notes

Reaction equation

HRID 1672315 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:11]=[CH:12][CH2:13][N+:14]([O-:16])=[O:15])=[C:6]([CH:10]=1)[C:7](O)=[O:8].C([O-])(=O)C.[K+]>C(OC(=O)C)(=O)C>[Cl:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:11]=[CH:12][C:13]([N+:14]([O-:16])=[O:15])=[C:7]2[OH:8]

Participants

4

Reactant 2

HCID 517044Potassium AcetateHCID 600469345-Chloro-2-(2-nitroethylideneamino)benzoic acid

Product 1

HCID 178526764HCID 178526764, compound

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

26.5 g (0.109 mol) of 5-chloro-2-[2-nitro-ethylideneamino]-benzoic acid (Example 23a) in 116 ml acetic anhydride are heated and kept at 110° C. 12.92 g (0.131 mol) potassium acetate are added in 2 min and heating is continued for 40 min at 130-135° C. After 10 min, the title compound starts to crystallize. The reaction vessel is cooled to rt and the solid filtered off and washed with acetic acid and water. Drying follows at 95° C. for 16 h (high vacuum). mp: 341-342° C. (dec.). MS: 225 (M++1); HPLC: tret=7.33 min (Grad 1).

Workup

  1. customkept at 110° C
  2. temperatureheating
  3. waitAfter 10 min

Sources & evidence

ORD record
ord-25ea7433ddc44a01b9f8496ceaa8fde7
Source dataset
uspto-grants-2011_08
Patent number
US07998972B2

Reaction notes

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