Ethyl Acetoacetate → HCID 178428858, compound

HRID 47423

Reaction equation

HRID 47423 reaction equation
[F:1][C:2]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:3]=1[NH2:4].[C:10](OCC)(=[O:15])[CH2:11][C:12]([CH3:14])=O>>[OH:15][C:10]1[C:5]2[C:3](=[C:2]([F:1])[CH:8]=[CH:7][C:6]=2[F:9])[N:4]=[C:12]([CH3:14])[CH:11]=1

Participants

3

Reactant 2

HCID 8868Ethyl AcetoacetateHCID 677752,5-Difluoroaniline

Product 1

HCID 178428858HCID 178428858, compound

Conditions

Temperature
180 °C

Procedure

A mixture of 2,5-difluoroaniline (10.0 g), ethyl acetoaceate (9.85 ml) and polyphosphoric acid (62 ml) were heated with stirring at 180° C. for 5 h. The mixture was cooled to room temperature and neutralised with dilute NH4OH/ice. The title compound precipitated and was separated by filtration to give compound identical spectroscopically with a sample prepared by the two stage process described above.

Workup

  1. temperaturewere heated
  2. customThe title compound precipitated
  3. customwas separated by filtration
  4. customto give compound identical spectroscopically with a sample
  5. customprepared by the two stage process

Sources & evidence

ORD record
ord-8b17e9aa18ed46d68e546c4fd480db74
Source dataset
uspto-grants-2004_03
Patent number
US06699879B1

Linked notes

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