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Water → HCID 22273086, compound

HRID 1064365
Notes
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Reaction equation

HRID 1064365 reaction equation
[Cl:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:5]([NH2:6])=[C:4]([F:12])[C:3]=1F.[N:14]1([CH2:20][CH2:21][OH:22])[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[Cl:1][C:2]1[C:3]([N:17]2[CH2:18][CH2:19][N:14]([CH2:20][CH2:21][OH:22])[CH2:15][CH2:16]2)=[C:4]([F:12])[C:5]([NH2:6])=[C:7]([N+:9]([O-:11])=[O:10])[CH:8]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 76771-(2-Hydroxyethyl)piperazineHCID 11430Potassium CarbonateHCID 178973294-Chloro-2,3-difluoro-6-nitroaniline

Product 1

HCID 22273086HCID 22273086, compoundYield 67.3%

Reagents, catalysts & solvents 1

HCID 679
Dimethyl Sulfoxide
Solvent

Conditions

Temperature
50 °C

Procedure

To a solution of 6.79 g of 4-chloro-2,3-difluoro-6-nitroaniline (which was synthesized following WO9856761 or WO9835977) and 4.70 g of 1-piperazine ethanol in 30 ml of dimethylsulfoxide, 9.23 g of potassium carbonate was added, followed by an hour's stirring at 50° C. After cooling the reaction liquid to room temperature, water was added thereto, followed by extraction with chloroform. The chloroform layer was dried on anhydrous magnesium sulfate, the solvent was distilled off and 6.98 g of the title compound in crude form was obtained as a yellow oily substance.

Workup

  1. waitfollowed by an hour
  2. temperatureAfter cooling
  3. customthe reaction liquid to room temperature
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe chloroform layer was dried on anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off

Sources & evidence

ORD record
ord-dd8929cfcc57458f93f3ea05beea15bc
Source dataset
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06969712B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes